SIMULTANEOUS DETERMINATION OF TELMISARTAN AND HYDROCHLOROTHIAZIDE IN TABLET DOSAGE FORM USING REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Save this PDF as:
 WORD  PNG  TXT  JPG

Size: px
Start display at page:

Download "SIMULTANEOUS DETERMINATION OF TELMISARTAN AND HYDROCHLOROTHIAZIDE IN TABLET DOSAGE FORM USING REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY"

Transcription

1 CHAPTER 5 SIMULTANEOUS DETERMINATION OF TELMISARTAN AND HYDROCHLOROTHIAZIDE IN TABLET DOSAGE FORM USING REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2 CHAPTER 5 Simultaneous determination of Telmisartan and Hydrochlorothiazide in tablet dosage form using reverse phase high performance liquid chromatography 5.0 INTRODUCTION The objective was to develop a single method for simultaneous determination of the Telmisartan and Hydrochlorothiazide tablet dosage form. The method, after development, was validated as per ICH guidelines Q2 (R1). The target for this research work was to present comprehensive methods of critical tests for each drug product. Thus this work can be treated as a monograph for the drug products. A brief introduction of each molecule is has already been included in the previous chapter. 5.1 LITERATURE SURVEY The literature survey reveals that, TE and HCTZ are reported in British Pharmacopoeia [6, 7]. There have been several publications describing analytical methods for the determination of HCTZ and TE individually or with other drugs as combination. However the finished product in combination dosage form was not official in any pharmacopeia (USP/ BP/ Comparisons of official methods available are compiled in tables and 5.1.2below. This search was performed at the start and during the course of the study. A draft monograph has been published in USP Forum Vol 36(3). The Monograph is now official as per USP 34, from December SPP SPTM, SVKM s NMIMS, Mumbai 85

3 Table 5.1.1: Assay Pharmacopeia methods for Drug Substance Method Telmisartan HCTZ BP 2011 USP 34 BP 2011 USP 34 Potentiometric Titration Potentiometric Titration Potentiometric Titration HPLC Column Not Applicable Not Applicable Not Applicable C18 50mm x 4.6mm: 3.5µ Column Temp Not Applicable Not Applicable Not Applicable 35 C Mobile Phase Not Applicable Not Applicable Not Applicable Solution A A mixture of acetonitrile and methanol (3:1) was prepared and degassed. Solution B A solution of anhydrous formic acid in water (5 in 1000) was prepared and degassed. SPP SPTM, SVKM s NMIMS, Mumbai 86

4 Gradient Not Applicable Not Applicable Not Applicable Time %A %B (min) Flow Rate Not Applicable Not Applicable Not Applicable 1ml/min Wavelength Not Applicable Not Applicable Not Applicable 275nm Inj Vol (µl) Not Applicable Not Applicable Not Applicable 10 SPP SPTM, SVKM s NMIMS, Mumbai 87

5 Table 5.1.2: Assay Pharmacopeia methods for Drug Product CHAPTER - 5 Telmisartan HCTZ Telmisartan-HCTZ BP 2011 USP 34 BP 2011 USP 34 USP 35 Method Not Available HPLC UV HPLC HPLC Spectrophotometer Column Not Applicable C18 40mm x 4.0mm; 5µ Not Applicable C18 250mm x 4.6mm; C8 125mm x 4.0mm; 5µ Column Not Applicable 40 C Not Applicable Not Mentioned 40 C Temp Mobile Phase Not Applicable Buffer g/l ammonium dihydrogen phosphate was prepared. ph was adjusted with 1 M phosphoric acid to 3.0 Mobile Phase: Methanol and Buffer (7:3) Not Applicable A degassed mixture of 0.1 M monobasic sodium phosphate and acetonitrile (9:1) was prepared. ph was adjusted with phosphoric acid to 3.0 ± 0.1 Buffer: 2.0 g/l of ammonium dihydrogen phosphate was prepared. ph was adjusted with phosphoric acid to 3.0. Solution A: Methanol and Acetonitrile (1:1) SPP SPTM, SVKM s NMIMS, Mumbai 88

6 Gradient Not Applicable Isocratic (Run time Not Applicable Isocratic (Run time Time %Buffer %Solution not mentioned) not mentioned) (min) A Flow Rate Not Applicable 0.7ml/min Not Applicable 2ml/min 1.2ml/min Wavelength Not Applicable 298nm 273nm 254nm 270-Telmisartan 298- HCTZ Inj Vol (µl) Not Applicable 5 Not Applicable SPP SPTM, SVKM s NMIMS, Mumbai 89

7 5.2 PRESENT WORK AND DISCUSSION Selection of Chromatographic Method Reverse Phase chromatography was the natural choice for method development because of its ease of handling and robust nature. All development was conducted using reverse phase methods. Official methods and methods published in literature for Telmisartan and Hydrochlorothiazide are based on reverse phase chromatographic (RPC) separation Selection of Stationary Phase USP, EP monograph and reported HPLC methods of Telmisartan or hydrochlorothiazide recommended use of C18 column for the purpose of determination of related impurities and assay. So C18 columns were preferred as stationary phase. However, one of the important criteria for assay method development was to have a short run time. Thus C8 columns were tried to reduce the retention of the major constituents Selection of Wavelength for Analysis The optimum wavelength selected was 270 nm which represents the wavelength where both components had suitable responses in order to permit simultaneous determination of Telmisartan and HCTZ. 270nm is also the wavelength which has absorption maxima for hydrochlorothiazide and absorption minima for Telmisartan. Thus at this wavelength, minor changes will not affect peak areas and thus the final result. This will in effect produce a robust method with respect to wavelength. Figure: Overlaid UV spectrum of Telmisartan and Hydrochlorothiazide SPP SPTM, SVKM s NMIMS, Mumbai 90

8 5.2.4 Selection and Optimization of Mobile Phase From the experience with the retentively of the molecules as discussed in the previous chapter, a gradient run was the only viable option for a shorter run time. A high aqueous percentage was used in the initial period to retain the hydrochlorothiazide while a higher organic was used to elute the Telmisartan in the later period. Similar to the method for related substances, it was decided to proceed with ion pair chromatography. For assay experiment the primary use of ion pair reagent would be to retain the Hydrochlorothiazide peak and separate it from its main degradant which would, otherwise, eluted very close or could merge with the main peak. Unlike in method for impurities, in an assay method it would not cause any problem if the impurities elute in dead volume. During development of an assay, one of the main selectivity (specificity) criteria is that the degradants should not co-elute with the main analyte peak. The current experiment, being a multi component one, had the additional challenge of ensuring that a degradant of one constituent does not interfere with the other constituent. In other words a degradants due to Hydrochlorothiazide should not interfere with the Telmisartan peak and vice versa. Optimized Chromatographic Conditions: Instruments/Equipment : HPLC, Make Waters, Alliance, 2695 Separation Module, (UV/PDA), or equivalent. Analytical Balance, Make Mettler Toledo, Model- XS205DU, or equivalent. Column : Inertsil C8-3, 150 x 4.6 mm, 5µm or equivalent Flow rate : 2.0 ml/minute Column temperature : 30 C Wavelength : 270 nm Sample temperature : 20 C Injection volume : 20 l Run time : 15 minutes Diluent : 0.1N Methanolic NaOH SPP SPTM, SVKM s NMIMS, Mumbai 91

9 Diluent: 0.1N Methanolic NaOH Weigh accurately and transfer 4 gm of Sodium hydroxide in 1000 ml volumetric flask and add 40 ml water, sonnicate to dissolve and make the volume with Methanol. Mobile Phase A (Buffer): Mix 2 ml of Triethylamine in 1000 ml water. Adjust ph 3.0 with ortho-phosphoric acid. Mobile Phase B: Acetonitrile Preparation of Mobile Phase use for dilution: Prepare a mixture of Buffer: Acetonitrile in the ratio 85:15 v/v/v. Mix and degas. Gradient Program: Time in minutes Mobile Phase (A) % Mobile Phase (B) % Mobile Phase A : Mix 2 ml of Triethylamine in 1000 ml water. Adjust ph 3.0 with ortho-phosphoric acid. Mobile Phase B : Acetonitrile SPP SPTM, SVKM s NMIMS, Mumbai 92

10 5.3 FORCED DEGRADATION STUDIES The forced degradation studies were carried out to achieve adequate degradation of the individual drugs. They were carried out on the higher strength tablets (80mg_12.5mg) and chromatographed along with a non-stressed sample (control). The placebo was treated similarly. Since the degradation probabilities of the individual drugs are very different from each other, the degradation conditions were kept different for target drug. Preparation of Sample stock solution: 10 tablets were transferred into 500ml volumetric flask. 300ml of diluent was added and sonnicated for 20 minutes; allowed to cool at room temperature. The volume was made up to the mark with diluent. Preparation of Placebo stock solution: Accurately weighed placebo similar to sample and transferred into 500ml volumetric flask. 300ml of diluent was added and sonnicated for 20 minutes; allowed to cool at room temperature. The volume was made up to the mark with diluent Hydrolytic conditions: acid-, base-induced degradation. Acid Induced degradation Telmisartan: 5ml of sample stock solution was transferred into 50 ml volumetric flask. 5 ml of 5N Hydrochloric acid was added. This solution was heated on the water bath at 70 C for 24 hours. This was cooled; neutralized with same volume and same strength alkali. This was made up the volume with diluent and filtered through 0.45 Nylon filter. Hydrochlorothiazide: 5ml of sample stock solution was transferred into 50 ml volumetric flask. 5 ml of 1N Hydrochloric acid was added. This solution was heated on the water bath at 70 C for 30 minutes. This was cooled; neutralized with same volume and same strength alkali. This was made up the volume with diluent and filtered through 0.45 Nylon filter. Placebo preparation: Placebos were prepared accordingly on the same lines with samples. SPP SPTM, SVKM s NMIMS, Mumbai 93

11 Base Induced degradation Telmisartan: 5ml of sample stock solution was transferred into 50 ml volumetric flask. 5 ml of 5N Sodium Hydroxide was added. This solution was heated in the oven at 70 C for 24 hours. This was cooled; neutralized with same volume and same strength acid. Made up the volume with diluent and filtered through 0.45 Nylon filter. Hydrochlorothiazide: 5ml of sample stock solution was transferred into 50 ml volumetric flask. 5 ml of 1N Sodium hydroxide was added. This solution was heated on the water bath at 70 C for 2 hours. This was cooled; neutralized with same volume and same strength acid. Made up the volume with diluent and filtered through 0.45 Nylon filter. Placebo preparation: Placebos were prepared accordingly on the same lines with samples Oxidative condition: hydrogen peroxide-induced degradation. Telmisartan and Hydrochlorothiazide: 5ml of sample stock solution was transferred into 50 ml volumetric flask. 5ml of 50% Hydrogen peroxide was added. This solution was heated in the oven at 70 C for 24 hours. This was cooled; made up the volume with diluent and filtered through 0.45 Nylon filter. Placebo preparation: Placebo was prepared accordingly on the same lines with samples Thermal degradation study. Telmisartan: 5ml of sample stock solution was transferred into 50 ml volumetric flask and heated at 70 C for 24 hours on the water bath. This was cooled; diluted up to the mark with diluent and filtered through 0.45 Nylon filter. SPP SPTM, SVKM s NMIMS, Mumbai 94

12 Hydrochlorothiazide: 5ml of sample stock solution was transferred into 50 ml volumetric flask and heated at 70 C for 2 minutes in an oven. This was cooled; diluted up to the mark with diluent and filtered through 0.45 Nylon filter. Placebo preparation: Placebos were prepared accordingly on the same lines with samples Photolytic degradation study. As per guidelines for photostability testing of new drug substances and products, samples should be exposed to light providing an overall illumination of not less than 1.2 million lx hours and an integrated near ultraviolet energy of not less than 200Wh/m2 to allow direct comparisons to be made between the drug substance and drug product. [19] 5.0ml of sample stock solution was exposed under UV and white light for 1.2 million lux hours in each of 50 ml of clear glass flask volumetric flask, amber colour 50 ml glass volumetric flask and flask covered with aluminium foil. This solution was diluted to 50 ml with diluent and filtered through 0.45 Nylon filter. Placebo preparation: Placebo was prepared accordingly on the same lines with samples Observations in forced degradation studies. Under all conditions the peak due to the actives were found to be pure. Telmisartan Telmisartan degrades significantly in acidic, thermal and oxidative conditions. The degradation is acid has already been discussed in the chapter on method for related substances, is due to the formation of Methanolic ester due to the presence of methanol in the diluent. The degradation observed is much higher when compared to the related substances method because of difference in concentration of analyte in solution and difference in the diluents. Thus, it is quite possible that the degradation had reached SPP SPTM, SVKM s NMIMS, Mumbai 95

13 secondary or tertiary stage. In other words, the impurities had also degraded further. However, primary concern in the assay method development is the peak purity of the main peak and the peak purity for the Telmisartan peak is comfortably passing in all cases. Hydrochlorothiazide Due to the already known fact of the instability of Hydrochlorothiazide, the degradation conditions were much milder than what Telmisartan was exposed to. Hydrochlorothiazide degraded in all conditions. However under photolytic conditions, where the conditions are predetermined as per ICH guidelines, the degradation was found to be major. Additionally it has to be understood that the solution stability for hydrochlorothiazide is low and storing the solution for a few days to allow it to be exposed to the necessary illumination had also contributed to the degradation. The impurity generated is very near to the main peak at this high level. Thus it is important to protect the solution from light. 5.4 EXPERIMENTAL WORK Instrumentation Equipment Make Model HPLC Waters 2695Alliance Separation Module, (PDA/UV Detector) 2996/2487 Column GL Sciences Inc. Inertsil C x 4.6 mm, 5µm ph meter Thermo Orion-4star Electron Corp. Analytical Balance Mettler Toledo XS205DU SPP SPTM, SVKM s NMIMS, Mumbai 96

14 5.4.2 Chemicals and Reagents Name Grade Manufacturer Triethylamine HPLC grade Merck Methanol Gradient grade Merck Acetonitrile Gradient grade Rankem Sodium Hydroxide GR Merck Ortho-phosphoric acid GR Merck Hydrochloric acid GR Merck Hydrogen peroxide GR Merck Water HPLC milli-q In-house Working Standard Working Standard: Standard Lot.No. Potency (as is) Telmisartan TE Hydrochlorothiazide HCT/ Test Sample: Batch. No. Label claim (mg/tablets) Telmisartan Hydrochlorothiazide THT/ / THT/ / Placebo: Batch. No. THT/ /034 P THT/ /034 PH THT/ /034 PT SPP SPTM, SVKM s NMIMS, Mumbai 97

15 5.4.4 Solution Preparation Preparation of Standard solution: Standard Stock solution-telmisartan Accurately weigh and transfer about 80.0 mg of Telmisartan standard and transfer into a 50 ml volumetric flask, add 30 ml of diluent, sonnicate to dissolve and make up the volume with diluent. Standard Stock solution-hydrochlorothiazide Accurately weigh and transfer about 50.0 mg of Hydrochlorothiazide standard and transfer into a 100 ml volumetric flask, add 70 ml of Acetonitrile, sonnicate to dissolve and make up the volume with Acetonitrile. Standard Solution: Take 5 ml of Standard Stock solution of Telmisartan and 5 ml of Standard Stock solution of Hydrochlorothiazide in 100 ml volumetric flask; make the volume with mobile phase. Preparation of Sample solution: For mg Weigh accurately 10 tablets and transfer these tablets into a 500ml volumetric flask. Add 300ml of diluent and sonnicate it for 20 minutes; allow it to cool at room temperature. Make up the volume up to the mark with diluent. Dilute 5 ml of this solution to 50 ml with mobile phase. Filter the sample solution through 0.45 Nylon filter. For mg Weigh accurately 10 tablets and transfer these tablets into 500ml volumetric flask. Add 300ml of diluent and sonnicate it for 20 minutes; allow it to cool at room temperature. Make up the volume up to the mark with diluent. Dilute 5 ml of this solution to 50 ml with mobile phase. Filter the sample solution through 0.45 Nylon filter. Preparation of Placebo solution: Weigh accurately placebo similar to the sample and transfer these into 500ml volumetric flask. Add 300ml of diluent and sonnicate it for 20 minutes; allow it to cool SPP SPTM, SVKM s NMIMS, Mumbai 98

16 at room temperature. Make up the volume up to the mark with diluent. Dilute 5 ml of this solution to 50 ml with mobile phase. Filter the sample solution through 0.45 Nylon filter. (Use placebo preparation for only Validation) Evaluation of System suitability: Inject the Standard solution five times; the relative standard deviation of five replicate injections should not be more than 2.0% for Telmisartan and Hydrochlorothiazide. The USP tailing factor for Telmisartan and Hydrochlorothiazide peak should not be more than 2.0. The USP plates for Hydrochlorothiazide and Telmisartan should not be less than 4000 and 10,000 respectively. Procedure: Inject equal volumes of Blank (diluent), Standard solution (5 replicate) and sample solution (duplicate). Calculation: Calculate the amount of Telmisartan and Hydrochlorothiazide present in the Tablets as per give For Telmisartan AT WS P % Assay = x x x x x AS Tab 5 LC For Hydrochlorothiazide AT WS P % Assay = x x x x x AS Tab 5 LC Where, AT = Area of peak due to Active Ingredient in sample preparation. AS = Area of peak due to Active Ingredient in standard preparation. WS = Weight of Active Ingredient standard in mg. LC = Label claim of Active Ingredient per tablet in mg. P = Potency of Active Ingredient standard on as is basis. SPP SPTM, SVKM s NMIMS, Mumbai 99

17 5.5 VALIDATION OF THE DEVELOPED METHOD Validation parameters and acceptance criteria The validation summary is given in the below table Table : The validation summary Sr.No Parameters Acceptance criteria Result obtained 1.0 System suitability Telmisartan HCTZ % RSD for Standard solution USP Tailing USP Plate count NMT 2.0% NMT 2.0 Hydrochlorothiazide -NLT Telmisartan-NLT 10, Specificity Identification Results should be comparable with respect to the retention Retention time (min) time. 2.2 Interference No interference from blank and placebo to main component. Complies 2.3 Peak purity Purity angle should be less than purity threshold. Sample Purity angle Purity Threshold Standard peak should be pure for working concentration level. Standard of Telmisartan Sample of Telmisartan Standard of HCTZ Sample of HCTZ SPP SPTM, SVKM s NMIMS, Mumbai 100

18 Table : The validation summary (continued) Sr.No. Parameters 2.4 Forced degradation 3.0 Linearity Acceptance criteria The peak due to Telmisartan and Hydrochlorothiazide should be pure as shown on the PDA. Response should be Linear Correlation coefficient should not be less than % Limit of Y- Intercept should be within ± 2.0% of the corresponding Y-co-ordinate of the working level. Result obtained Telmisartan Condition % Purity Purity Assay angle Threshold Control Acid Base Peroxide Heat Photolytic Hydrochlorothiazide Control Acid Base Peroxide Heat Photolytic Response is linear Telmisartan 80 mg 40 mg HCTZ % -0.03% 0.88% SPP SPTM, SVKM s NMIMS, Mumbai 101

19 Table : The validation summary (continued) Sr. No Parameters Acceptance criteria Result obtained 4.0 Accuracy (Recovery) Precision System Precision % RSD for Standard sol USP Tailing USP Plate count 5.2 Method Precision % RSD of six determinations Intermediate Precision (Ruggedness) % RSD for Standard sol Mean recovery should be in the range of 98.0% %. NMT 2.0% Level % NMT 2.0 Hydrochlorothiazide -NLT Telmisartan-NLT 10,000. % Mean Recovery 80mg Telmisartan 40mg HCTZ Telmisartan HCTZ NMT 2.0%. For 80 mg Tablets NMT 2.0%. For 40 mg Tablets NMT 2.0% USP Tailing NMT USP Plate count Hydrochlorothiazide NLT Telmisartan-NLT 10, RSD for % Assay NMT 2.0%. For 80 mg Tablets NMT 2.0%. For 40 mg Tablets Difference in pooled result ( Analyst-I and II ) The difference in the means should not be more than mg mg SPP SPTM, SVKM s NMIMS, Mumbai 102

20 Table : The validation summary (continued) Sr. No. Parameters Acceptance criteria Result obtained 6.0 Stability in analytical solution Filter 7.0 compatibility Robustness Change in Flow rate (± 0.2 ml/min) The % difference should not be more than 2. The % difference between centrifuged sample and filtered sample should not be more than 2. No significant change should be in System suitability parameters. % RSD should be less than 2%. Telmisartan HCTZ Sample is Sample is stable upto stable upto hours, hours, stored stored at at 20 C. 20 C. Complies Complies No significant change. Compiles 8.0 Change in wavelength (± 5nm) No significant change should be in System suitability parameters. % RSD should be less than 2%. No significant change. Compiles Change in Buffer ph (± 0.2) Column oven temperature (± 5 C) No significant change should be in System suitability parameters. % RSD should be less than 2%. No significant change should be in System suitability parameters. % RSD should be less than 2%. No significant change. Compiles No significant change. Compiles SPP SPTM, SVKM s NMIMS, Mumbai 103

21 5.5.2 System suitability: Single injection of Blank (Diluent) and five replicate Standard solution were made on the system. The data obtained is summarized in Table The data demonstrate that the system suitability is within the acceptance criteria, thus the system is suitable. Table : System suitability Telmisartan Hydrochlorothiazide USP Tailing USP Plates Standard solution Area Mean SD %RSD Specificity: The Specificity study included Identification of the main peak, Interference study and Peak Purity. Peak purity of degraded peak was also studied. Injections of standard solution, sample solution and placebo, as a directed in experimental section, were made onto the HPLC. The data demonstrate that there is no interference in blank and placebo peaks with the peaks due to Telmisartan and Hydrochlorothiazide. Purity angle is less than purity threshold for the main peaks. The data obtained is summarized in Table Table : Specificity (Identification and Interference) Component Retention time (min) USP Plates USP Tailing Purity angle Purity threshold Standard solution Hydrochlorothiazide Telmisartan Sample solution Hydrochlorothiazide Telmisartan SPP SPTM, SVKM s NMIMS, Mumbai 104

22 Chromatograms of Blank (diluent), placebos, Standard solution and Sample solution are given below under n to Figure : Chromatogram of Blank. Figure : Chromatogram of Placebo without Telmisartan and Hydrochlorothiazide. SPP SPTM, SVKM s NMIMS, Mumbai 105

23 Figure : Chromatogram of Placebo with Telmisartan. Figure : Chromatogram of Placebo with Hydrochlorothiazide. SPP SPTM, SVKM s NMIMS, Mumbai 106

24 Figure : Chromatogram of Standard solution. Figure : Chromatogram of Sample solution. SPP SPTM, SVKM s NMIMS, Mumbai 107

25 Forced degradation: Under all degradation conditions, the peaks due to Telmisartan and Hydrochlorothiazide were found to be pure Linearity and Range: The Linearity of response was determined by preparing different concentrations of standard stock solution ranging from 50% to 150% of the working concentration. The data shows that the response is found to be linear; Correlation coefficient is more than The data summarized in Table , and Table : Linearity of Telmisartan (80 mg). Level Concentration (%) Response 1 2 Mean CORRELATION COEFFICIENT (r) SLOPE Y-INTERCEPT MEDIAN (AREA) % LIMIT OF Y-INTERCEPT ± 2% OF MEDIAN 0.80 SPP SPTM, SVKM s NMIMS, Mumbai 108

26 Table : Linearity of Telmisartan (40 mg). Level Concentration (%) Response 1 2 Mean CORRELATION COEFFICIENT (r) SLOPE Y-INTERCEPT -319 MEDIAN (AREA) % LIMIT OF Y-INTERCEPT ± 2% OF MEDIAN Table : Linearity of Hydrochlorothiazide. Level Concentration (%) Response 1 2 Mean CORRELATION COEFFICIENT (r) SLOPE 9286 Y-INTERCEPT 8271 MEDIAN (AREA) % LIMIT OF Y-INTERCEPT ± 2% OF MEDIAN 0.88 SPP SPTM, SVKM s NMIMS, Mumbai 109

27 Graph of concentration v/s area is attached as Figure , and Figure : Linearity for Telmisartan (80mg). Figure : Linearity for Telmisartan (40mg). SPP SPTM, SVKM s NMIMS, Mumbai 110

28 Figure : Linearity for Hydrochlorothiazide Accuracy: The standard solution was spiked into the placebo at three different level, 50%, 100% and 150% from three different standard stock solutions and each level in duplicate were injected. From the amount added and the amount found, the percentage recovery was calculated. The results obtained are summarized in Table to The data shows that the % mean recovery at each level is within the acceptance criteria. Table : % Recovery for Telmisartan (80 mg) Level Mean % Mean recovery % response Recovery % 50 % 100 % 150 % SPP SPTM, SVKM s NMIMS, Mumbai 111

29 Table : % Recovery for Telmisartan (40 mg) Level Mean % Mean recovery % response Recovery % 50 % 100 % 150 % Table : % Recovery for Hydrochlorothiazide. Level % Mean response % Recovery Mean recovery % 50 % 100 % 150 % SPP SPTM, SVKM s NMIMS, Mumbai 112

30 5.5.6 Precision System Precision: Single injection of Blank (Diluent) and five replicate injections of standard solution were made on the system. Please refer to Table for system suitability of mg strength. Table depicts the system suitability for strength. All the data were acceptable as per the system suitability requirements. Table : System precision (40/12.5 mg Tablets) Telmisartan Hydrochlorothiazide USP Tailing USP Plates Standard solution Area Mean SD %RSD Method Precision: Six sample solutions were prepared and injected in duplicate on the HPLC. The data obtained is summarized in Table and The data shows that % RSD is well within the acceptance criteria. SPP SPTM, SVKM s NMIMS, Mumbai 113

31 Table 14: Method precision (80/12.5 mg Tablets) Spl. No. Telmisartan Hydrochlorothiazide Response % Response % 1 2 Mean Assay 1 2 Mean Assay Mean SD % RSD Table 15: Method precision (40/12.5 mg Tablets) Spl. No. Telmisartan Hydrochlorothiazide Response % Response % 1 2 Mean Assay 1 2 Mean Assay Mean SD % RSD SPP SPTM, SVKM s NMIMS, Mumbai 114

32 Intermediate Precision (Ruggedness): Same procedure of system precision and method precision is followed by another Analyst on different instrument and on different day. The system suitability data obtained from Analyst-II are summarized in Table and The data demonstrate that the system complies. Thus the system was suitable and precise and % RSD is within the acceptance criteria. Table : System suitability (80/12.5 mg Tablets) Telmisartan Hydrochlorothiazide USP Tailing USP Plates Standard solution Area Mean SD %RSD Table : System suitability (40/12.5 mg Tablets) Telmisartan Hydrochlorothiazide USP Tailing USP Plates Standard solution Area Mean SD %RSD SPP SPTM, SVKM s NMIMS, Mumbai 115

33 The Data obtained by second analyst is given in table and The values are within acceptable limits. Table : Intermediate precision (80/12.5 mg Tablets) Spl. No. Telmisartan Hydrochlorothiazide Response % Response % 1 2 Mean Assay 1 2 Mean Assay Mean SD % RSD Table : Intermediate precision (40/12.5 mg Tablets) Spl. No. Telmisartan Hydrochlorothiazide Response % Response % 1 2 Mean Assay 1 2 Mean Assay Mean SD % RSD SPP SPTM, SVKM s NMIMS, Mumbai 116

34 The pooled data of twelve independent sample preparation obtained from Analyst-I and Analyst- II is summarized in Table and The results demonstrated that the values are within acceptable limits. Table : Pooled data (80/12.5 mg Tablets) Analyst Telmisartan % Assay Hydrochlorothiazide I Mean II Mean % Difference between two means SPP SPTM, SVKM s NMIMS, Mumbai 117

35 Table : Pooled data (40/12.5 mg Tablets) Analyst Telmisartan % Assay Hydrochlorothiazide I Mean II Mean % Difference between two means Stability in Analytical solution: The standard solution and sample solution were kept at sample temperature for 24 hours and were injected on to the HPLC time to time. The data obtained are summarized in Table and The data demonstrates that while Telmisartan sample solution was stable for at least 15 hours at the sample temperature, hydrochlorothiazide was stable for 24 hours. It was noted that the peak areas slowly increased over time. This suggested that there was slow evaporation of the solvent present in the diluent. SPP SPTM, SVKM s NMIMS, Mumbai 118

36 Table Stability in analytical solution (Telmisartan) Time Mean area of standard Cumulative RSD for % Assay % Difference solution standard area Initial (control) hrs hrs hrs hrs hrs Table Stability in analytical solution (Hydrochlorothiazide) Time Mean area of standard Cumulative RSD for % Assay % Difference solution standard area Initial (control) hrs hrs hrs hrs hrs Filter Compatibility: The Sample solution centrifuged and filtered through different filters was injected on to the HPLC. The data obtained are summarized in Table The data shows that % difference is not more than 2. Thus all filters tested were compatible with the sample. SPP SPTM, SVKM s NMIMS, Mumbai 119

37 Table Filter compatibility Filter Telmisartan Hydrochlorothiazide % Assay % Difference % Assay % Difference Centrifuged Glass Filter Nylon Filter Nylon + Glass Filter PVDF Teflon Teflon + Glass Filter Robustness: The changes in system suitability parameters and results, when deliberate controlled changes were made to the method, were studied in robustness. No significant changes in system suitability parameters or results were observed during robustness study proving the method to be considerable robust. The data obtained are summarized in Table and Table : Robustness (Telmisartan). Changes in parameters Values Retention time of Telmisartan USP Plates USP Tailing % RSD of standard area % Assay Cumulative % RSD Control As per method Flow rate (ml/min) Wavelength (nm) Column temperature ( C) Buffer ph SPP SPTM, SVKM s NMIMS, Mumbai 120

38 Table : Robustness (Hydrochlorothiazide). Changes in parameters Values Retention time of HCTZ USP Plates USP Tailing % RSD of standard area % Assay Cumulative % RSD Control As per method Flow rate (ml/min) Wavelength (nm) Column temperature ( C) Buffer ph Conclusions: The method has been shown to be specific for Telmisartan and Hydrochlorothiazide Tablets. The method has been shown to be Linear, precise and accurate across the suitable analytical range and stability indicating. Solution has been shown to be stable for at least 24 hours when stored at 20 C. The method has been shown to be robust towards deliberate minor changes in the method parameters. The method can be used in quality control laboratory for release of production batches. SPP SPTM, SVKM s NMIMS, Mumbai 121

Reversed Phase High Presssure Liquid Chromatograhphic Technique for Determination of Sodium Alginate from Oral Suspension

Reversed Phase High Presssure Liquid Chromatograhphic Technique for Determination of Sodium Alginate from Oral Suspension International Journal of PharmTech Research CODEN (USA): IJPRIF ISSN : 0974-4304 Vol.2, No.2, pp 1634-1638, April-June 2010 Reversed Phase High Presssure Liquid Chromatograhphic Technique for Determination

More information

Tamsulosin Hydrochloride Capsules

Tamsulosin Hydrochloride Capsules . nal Revision Bulletin Official October 1, 2011 Tamsulosin 1 standard solution, and shake well. Centrifuge at 1500 rpm for 10 min, and use the supernatant, passing it if Tamsulosin Hydrochloride Capsules

More information

SUCRALOSE. White to off-white, practically odourless crystalline powder

SUCRALOSE. White to off-white, practically odourless crystalline powder SUCRALOSE Prepared at the 41st JECFA (1993), published in FNP 52 Add 2 (1993). Metals and arsenic specifications revised at the 63rd JECFA (2004). An ADI of 0-15 mg/kg bw was established at the 37th JECFA

More information

Step-by-Step Analytical Methods Validation and Protocol in the Quality System Compliance Industry

Step-by-Step Analytical Methods Validation and Protocol in the Quality System Compliance Industry Step-by-Step Analytical Methods Validation and Protocol in the Quality System Compliance Industry BY GHULAM A. SHABIR Introduction Methods Validation: Establishing documented evidence that provides a high

More information

Development of validated RP- HPLC method for estimation of rivaroxaban in pharmaceutical formulation

Development of validated RP- HPLC method for estimation of rivaroxaban in pharmaceutical formulation IJPAR Vol.4 Issue 4 Oct Dec - 2015 Journal Home page: ISSN: 2320-2831 Research Article Open Access Development of validated RP- HPLC method for estimation of rivaroxaban in pharmaceutical formulation V.

More information

ANALYTICAL METHODS INTERNATIONAL QUALITY SYSTEMS

ANALYTICAL METHODS INTERNATIONAL QUALITY SYSTEMS VALIDATION OF ANALYTICAL METHODS 1 GERT BEUVING INTERNATIONAL PHARMACEUTICAL OPERATIONS TASKS: - Internal auditing - Auditing of suppliers and contract manufacturers - Preparing for and guiding of external

More information

Research Article. Stress study and estimation of a potent anticoagulant drug rivaroxaban by a validated HPLC method: Technology transfer to UPLC

Research Article. Stress study and estimation of a potent anticoagulant drug rivaroxaban by a validated HPLC method: Technology transfer to UPLC Available online www.jocpr.com Journal of Chemical and Pharmaceutical Research, 2015, 7(10):65-74 Research Article ISSN : 0975-7384 CODEN(USA) : JCPRC5 Stress study and estimation of a potent anticoagulant

More information

Analytical Test Report

Analytical Test Report Analytical Test Report Customer: Address (City, State): Purchase Order: Report Number: Project Number: Date Received: Date of Report: Test Location: Boulder, CO. Assay: Part Number: Amino Acids by HPLC

More information

LUMEFANTRINE Draft proposal for The International Pharmacopoeia (October 2006)

LUMEFANTRINE Draft proposal for The International Pharmacopoeia (October 2006) October 2006 RESTRICTED LUMEFANTRINE Draft proposal for The International Pharmacopoeia (October 2006) DRAFT FOR DISCUSSION World Health Organization 2006 All rights reserved. This draft is intended for

More information

ERDOSTEINE - MONOGRAPH.

ERDOSTEINE - MONOGRAPH. STRUCTURAL FORMULA (±1S-(2-[N-3-(2-oxotetrahydro thienyl)]acetamido)-thioglycolic acid) C 8 H 11 NO 4 S 2 M.W. = 249.307 DESCRIPTION Color : White to ivory white Appearance : Microcrystalline powder SOLUBILITY

More information

HPLC Analysis of Acetaminophen Tablets with Waters Alliance and Agilent Supplies

HPLC Analysis of Acetaminophen Tablets with Waters Alliance and Agilent Supplies HPLC Analysis of Acetaminophen Tablets with Waters Alliance and Agilent Supplies Application Note Small Molecule Pharmaceuticals Authors Jignesh Shah, Tiantian Li, and Anil Sharma Agilent Technologies,

More information

INTERNATIONAL JOURNAL OF PHARMACEUTICAL RESEARCH AND BIO-SCIENCE

INTERNATIONAL JOURNAL OF PHARMACEUTICAL RESEARCH AND BIO-SCIENCE Rajgor VM,, 2014; Volume 3(3): 188-197 INTERNATIONAL JOURNAL OF PHARMACEUTICAL RESEARCH AND BIO-SCIENCE ANALYTICAL METHOD DEVELOPEMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF MEMANTINE HCL AND

More information

Simultaneous determination of L-ascorbic acid and D-iso-ascorbic acid (erythorbic acid) in wine by HPLC and UV-detection (Resolution Oeno 11/2008)

Simultaneous determination of L-ascorbic acid and D-iso-ascorbic acid (erythorbic acid) in wine by HPLC and UV-detection (Resolution Oeno 11/2008) Method OIV-MA-AS313-22 Type II method Simultaneous determination of L-ascorbic acid and D-iso-ascorbic acid (erythorbic acid) in wine by HPLC and UV-detection (Resolution Oeno 11/2008) 1. Introduction

More information

Minor editorial changes have been made to update the monograph to the current USP style.

Minor editorial changes have been made to update the monograph to the current USP style. Amlodipine, Valsartan and Hydrochlorothiazide Tablets Type of Posting Revision Bulletin Posting Date 27 May 2016 Official Date 01 Jun 2016 Expert Committee Chemical Medicines Monographs 2 Reason for Revision

More information

Drospirenone and Ethinyl Estradiol Tablets. Type of Posting. Revision Bulletin Posting Date. 31 July 2015 Official Date

Drospirenone and Ethinyl Estradiol Tablets. Type of Posting. Revision Bulletin Posting Date. 31 July 2015 Official Date Drospirenone and Ethinyl Estradiol Tablets Type of Posting Revision Bulletin Posting Date 31 July 2015 Official Date 01 August 2015 Expert Committee MonographsSmall Molecules 4 Reason for Revision Compliance

More information

Guidance for Industry

Guidance for Industry Guidance for Industry Q2B Validation of Analytical Procedures: Methodology November 1996 ICH Guidance for Industry Q2B Validation of Analytical Procedures: Methodology Additional copies are available from:

More information

VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY Q2(R1)

VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY Q2(R1) INTERNATIONAL CONFERENCE ON HARMONISATION OF TECHNICAL REQUIREMENTS FOR REGISTRATION OF PHARMACEUTICALS FOR HUMAN USE ICH HARMONISED TRIPARTITE GUIDELINE VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY

More information

Develop a Quantitative Analytical Method for low (» 1 ppm) levels of Sulfate

Develop a Quantitative Analytical Method for low (» 1 ppm) levels of Sulfate Cantaurus, Vol. 7, 5-8, May 1999 McPherson College Division of Science and Technology Develop a Quantitative Analytical Method for low (» 1 ppm) levels of Sulfate Janet Bowen ABSTRACT Sulfate is used in

More information

International Journal of Pharma and Bio Sciences V1(2)2010

International Journal of Pharma and Bio Sciences V1(2)2010 1 Central Drugs Laboratory,Kolkata Angshuman Biswas 1 and Arindam Basu 1 *Corresponding author bangshuman@rediffmail.com ABSTRACT A fast and reliable high performance liquid chromatography method for determination

More information

Analytical Test Method Validation Report Template

Analytical Test Method Validation Report Template Analytical Test Method Validation Report Template 1. Purpose The purpose of this Validation Summary Report is to summarize the finding of the validation of test method Determination of, following Validation

More information

Quality by Design Approach for the Separation of Naproxcinod and its Related Substances by Fused Core Particle Technology Column

Quality by Design Approach for the Separation of Naproxcinod and its Related Substances by Fused Core Particle Technology Column Journal of Chromatographic Science Advance Access published October 11, 2012 Journal of Chromatographic Science 2012;00:1 7 doi:10.1093/chromsci/bms162 Article Quality by Design Approach for the Separation

More information

Journal of Chemical and Pharmaceutical Research

Journal of Chemical and Pharmaceutical Research Available on line www.jocpr.com Journal of Chemical and Pharmaceutical Research ISSN No: 0975-7384 CODEN(USA): JCPRC5 J. Chem. Pharm. Res., 2010, 2(6):62-67 Development and validation of RP- HPLC method

More information

CONFIRMATION OF ZOLPIDEM BY LIQUID CHROMATOGRAPHY MASS SPECTROMETRY

CONFIRMATION OF ZOLPIDEM BY LIQUID CHROMATOGRAPHY MASS SPECTROMETRY CONFIRMATION OF ZOLPIDEM BY LIQUID CHROMATOGRAPHY MASS SPECTROMETRY 9.1 POLICY This test method may be used to confirm the presence of zolpidem (ZOL), with diazepam-d 5 (DZP-d 5 ) internal standard, in

More information

Journal of Chemical and Pharmaceutical Research

Journal of Chemical and Pharmaceutical Research Available on line www.jocpr.com Journal of Chemical and Pharmaceutical Research J. Chem. Pharm. Res., 2010, 2(1): 91-99 ISSN No: 0975-7384 A Stability-Indicating RP-LC method for the Determination of Related

More information

Journal of Chemical and Pharmaceutical Research, 2012, 4(6):3263-3274. Research Article

Journal of Chemical and Pharmaceutical Research, 2012, 4(6):3263-3274. Research Article Available online www.jocpr.com Journal of Chemical and Pharmaceutical Research, 2012, 4(6):3263-3274 Research Article ISSN : 0975-7384 CODEN(USA) : JCPRC5 Impurities profiling Method and degradation studies

More information

PVV Satyanaryana et al., IJSID, 2012, 2 (1), 226-231. International Journal of Science Innovations and Discoveries

PVV Satyanaryana et al., IJSID, 2012, 2 (1), 226-231. International Journal of Science Innovations and Discoveries ISSN:2249-5347 IJSID International Journal of Science Innovations and Discoveries An International peer Review Journal for Science Research Article Available online through www.ijsidonline.info RP-HPLC

More information

A NEW METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF RIVAROXABAN IN FORMULATION BY RP HPLC

A NEW METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF RIVAROXABAN IN FORMULATION BY RP HPLC A NEW METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF RIVAROXABAN IN FORMULATION BY RP HPLC K.Chandra sekhar, P. Satya vani, A. Dhana lakshmi, Ch.LL.Devi, Anupama Barik, Narendra Devanaboyina * Department

More information

Application Note. Determination of Nitrite and Nitrate in Fruit Juices by UV Detection. Summary. Introduction. Experimental Sample Preparation

Application Note. Determination of Nitrite and Nitrate in Fruit Juices by UV Detection. Summary. Introduction. Experimental Sample Preparation Application Note Determination of Nitrite and Nitrate in Fruit Juices by UV Detection Category Food Matrix Fruit Juice Method HPLC Keywords Ion pair chromatography, fruit juice, inorganic anions AZURA

More information

VALIDATION OF HPLC METHOD FOR DETERMINATION OF DOCOSAHEXAENOIC ACID (DHA) IN MULIIVITAMIN CAPSULE DIAH WIDOWATI*, ROS SUMARNY, ESTI MUMPUNI

VALIDATION OF HPLC METHOD FOR DETERMINATION OF DOCOSAHEXAENOIC ACID (DHA) IN MULIIVITAMIN CAPSULE DIAH WIDOWATI*, ROS SUMARNY, ESTI MUMPUNI VALIDATION OF HPLC METHOD FOR DETERMINATION OF DOCOSAHEXAENOIC ACID (DHA) IN MULIIVITAMIN CAPSULE DIAH WIDOWATI*, ROS SUMARNY, ESTI MUMPUNI Fakultas Farmasi Universitas Pancasila Jln. Srengseng Sawah,

More information

α-cyclodextrin SYNONYMS α-schardinger dextrin, α-dextrin, cyclohexaamylose, cyclomaltohexaose, α- cycloamylase

α-cyclodextrin SYNONYMS α-schardinger dextrin, α-dextrin, cyclohexaamylose, cyclomaltohexaose, α- cycloamylase α-cyclodextrin New specifications prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001). An ADI not specified was established at the 57th JECFA (2001). SYNONYMS α-schardinger dextrin,

More information

High Performance Thin Layer Chromatographic Method for Estimation of Cefprozil in Tablet Dosage Form

High Performance Thin Layer Chromatographic Method for Estimation of Cefprozil in Tablet Dosage Form ISSN: 0973-4945; CODEN ECJHAO E- Chemistry http://www.e-journals.net Vol. 5, No.3, pp. 427-430, July 2008 High Performance Thin Layer Chromatographic Method for Estimation of Cefprozil in Tablet Dosage

More information

Simultaneous determination of aspartame, benzoic acid, caffeine, and saccharin in sugar-free beverages using HPLC

Simultaneous determination of aspartame, benzoic acid, caffeine, and saccharin in sugar-free beverages using HPLC Simultaneous determination of aspartame, benzoic acid, caffeine, and saccharin in sugar-free beverages using HPLC Mackenzie Ree and Erik Stoa Department of Chemistry, Concordia College, 901 8 th St S,

More information

Validation and Calibration of Analytical Instruments a D.Gowrisankar, b K.Abbulu, c O.Bala Souri, K.Sujana*

Validation and Calibration of Analytical Instruments a D.Gowrisankar, b K.Abbulu, c O.Bala Souri, K.Sujana* Validation and Calibration of Analytical Instruments a D.Gowrisankar, b K.Abbulu, c O.Bala Souri, K.Sujana* a Department of Pharmaceutical Analysis, Andhra University, Visakhapatnam. b Department of Pharmaceutics,

More information

Rao, et al., Int J Res Pharm Sci 2015, 5(2) ; 17 24. Available online at www.ijrpsonline.com. Research Article

Rao, et al., Int J Res Pharm Sci 2015, 5(2) ; 17 24. Available online at www.ijrpsonline.com. Research Article International Journal of Research in Pharmacy and Science Available online at www.ijrpsonline.com Research Article Stability-indicating UPLC method for determining related substances and degradants in

More information

ANALYTICAL METHOD DEVELOPMENT FOR DISSOLUTION RELEASE OF FINISHED SOLID ORAL DOSAGE FORMS

ANALYTICAL METHOD DEVELOPMENT FOR DISSOLUTION RELEASE OF FINISHED SOLID ORAL DOSAGE FORMS Academic Sciences International Journal of Current Pharmaceutical Research ISSN- 0975-7066 Vol 4, Issue 2, 2012 Research Article ANALYTICAL METHOD DEVELOPMENT FOR DISSOLUTION RELEASE OF FINISHED SOLID

More information

ICH Topic Q 2 (R1) Validation of Analytical Procedures: Text and Methodology. Step 5

ICH Topic Q 2 (R1) Validation of Analytical Procedures: Text and Methodology. Step 5 European Medicines Agency June 1995 CPMP/ICH/381/95 ICH Topic Q 2 (R1) Validation of Analytical Procedures: Text and Methodology Step 5 NOTE FOR GUIDANCE ON VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND

More information

A Complete Solution for Method Linearity in HPLC and UHPLC

A Complete Solution for Method Linearity in HPLC and UHPLC Now sold under the Thermo Scientific brand A Complete Solution for Method Linearity in HPLC and UHPLC Frank Steiner, Fraser McLeod, Tobias Fehrenbach, and Andreas Brunner Dionex Corporation, Germering,

More information

Transfer of a USP method for prednisolone from normal phase HPLC to SFC using the Agilent 1260 Infinity Hybrid SFC/UHPLC System Saving time and costs

Transfer of a USP method for prednisolone from normal phase HPLC to SFC using the Agilent 1260 Infinity Hybrid SFC/UHPLC System Saving time and costs Agilent Application Solution Transfer of a USP method for prednisolone from normal phase PLC to SFC using the Agilent 126 Infinity ybrid SFC/UPLC System Saving time and costs Application Note Pharmaceutical

More information

Project 5: Scoville Heat Value of Foods HPLC Analysis of Capsaicinoids

Project 5: Scoville Heat Value of Foods HPLC Analysis of Capsaicinoids Willamette University Chemistry Department 2013 Project 5: HPLC Analysis of Capsaicinoids LABORATORY REPORT: Formal Writing Exercises PRE-LAB ASSIGNMENT Read the entire laboratory project and section 28C

More information

Automated Method Development Utilizing Software-Based Optimization and Direct Instrument Control

Automated Method Development Utilizing Software-Based Optimization and Direct Instrument Control Automated Method Development Utilizing Software-Based Optimization and Direct Instrument Control Dr. Frank Steiner, 1 Andreas Brunner, 1 Fraser McLeod, 1 Dr. Sergey Galushko 2 1 Dionex Corporation, Germering,

More information

ETHYL LAUROYL ARGINATE

ETHYL LAUROYL ARGINATE ETHYL LAURYL ARGINATE New specifications prepared at the 69th JECFA (2008), published in FA JECFA Monographs 5 (2008). An ADI of 0-4 mg/kg bw was established at the 69th JECFA (2008). SYNNYMS DEFINITIN

More information

DRAFT MONOGRAPH FOR THE INTERNATIONAL PHARMACOPOEIA PARACETAMOL ORAL SUSPENSION (September 2010)

DRAFT MONOGRAPH FOR THE INTERNATIONAL PHARMACOPOEIA PARACETAMOL ORAL SUSPENSION (September 2010) September 2010 RESTRICTED DRAFT MONOGRAPH FOR THE INTERNATIONAL PHARMACOPOEIA PARACETAMOL ORAL SUSPENSION (September 2010) DRAFT FOR COMMENTS This document was provided by a quality control expert and

More information

LC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research

LC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research LC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research J. Jones, J. Denbigh, Thermo Fisher Scientific, Runcorn, Cheshire, UK Application Note 20581 Key Words SPE, SOLA,

More information

Analysis of Various Vitamins in Multivitamin Tablets

Analysis of Various Vitamins in Multivitamin Tablets High Performance Liquid Chromatography Analysis of Various Vitamins in Multivitamin Tablets Effective August 24, 2007, the US Food and Drug Administration (FDA) issued a regulation (21 CFR Part 111) that

More information

The Theory of HPLC. Gradient HPLC

The Theory of HPLC. Gradient HPLC The Theory of HPLC Gradient HPLC i Wherever you see this symbol, it is important to access the on-line course as there is interactive material that cannot be fully shown in this reference manual. Aims

More information

GUIDELINES FOR THE VALIDATION OF ANALYTICAL METHODS FOR ACTIVE CONSTITUENT, AGRICULTURAL AND VETERINARY CHEMICAL PRODUCTS.

GUIDELINES FOR THE VALIDATION OF ANALYTICAL METHODS FOR ACTIVE CONSTITUENT, AGRICULTURAL AND VETERINARY CHEMICAL PRODUCTS. GUIDELINES FOR THE VALIDATION OF ANALYTICAL METHODS FOR ACTIVE CONSTITUENT, AGRICULTURAL AND VETERINARY CHEMICAL PRODUCTS October 2004 APVMA PO Box E240 KINGSTON 2604 AUSTRALIA http://www.apvma.gov.au

More information

TANNIC ACID. SYNONYMS Tannins (food grade), gallotannic acid, INS No. 181 DEFINITION DESCRIPTION

TANNIC ACID. SYNONYMS Tannins (food grade), gallotannic acid, INS No. 181 DEFINITION DESCRIPTION TANNIC ACID Prepared at the 39th JECFA (1992), published in FNP Add 1 (1992) superseding specifications prepared at the 35th JECFA (1989), published in FNP 49 (1990) and in FNP 52 (1992). Metals and arsenic

More information

Thermo Scientific Syncronis HPLC Columns. Technical Manual

Thermo Scientific Syncronis HPLC Columns. Technical Manual Thermo Scientific Syncronis HPLC Columns Technical Manual Thermo Scientific Syncronis HPLC Columns When developing a new method, one of the most important goals for the chromatographer is to achieve a

More information

Analysis of Free Bromate Ions in Tap Water using an ACQUITY UPLC BEH Amide Column

Analysis of Free Bromate Ions in Tap Water using an ACQUITY UPLC BEH Amide Column Analysis of Free Bromate Ions in Tap Water using an ACQUITY UPLC BEH Amide Column Sachiki Shimizu, FUJIFILM Fine Chemicals Co., Ltd., Kanagawa, Japan Kenneth J. Fountain, Kevin Jenkins, and Yoko Tsuda,

More information

ACETALDEHYDE and ISOVALERALDEHYDE (Gas Chromatography)

ACETALDEHYDE and ISOVALERALDEHYDE (Gas Chromatography) ACETA.02-1 ACETALDEHYDE and ISOVALERALDEHYDE (Gas Chromatography) PRINCIPLE Isovaleraldehyde (IVA) and acetaldehyde are released from the syrup with the aid of dilute phosphoric acid and heat. The liberated

More information

Standard Operating Procedure for Total Kjeldahl Nitrogen (Lachat Method)

Standard Operating Procedure for Total Kjeldahl Nitrogen (Lachat Method) Standard Operating Procedure for Total Kjeldahl Nitrogen (Lachat Method) Grace Analytical Lab 536 South Clark Street 10th Floor Chicago, IL 60605 April 15, 1994 Revision 2 Standard Operating Procedure

More information

Guide to Reverse Phase SpinColumns Chromatography for Sample Prep

Guide to Reverse Phase SpinColumns Chromatography for Sample Prep Guide to Reverse Phase SpinColumns Chromatography for Sample Prep www.harvardapparatus.com Contents Introduction...2-3 Modes of Separation...4-6 Spin Column Efficiency...7-8 Fast Protein Analysis...9 Specifications...10

More information

Extraction of Cannabinoids in Marijuana and Edibles by QuEChERS

Extraction of Cannabinoids in Marijuana and Edibles by QuEChERS Extraction of Cannabinoids in Marijuana and Edibles by QuEChERS UCT Part Numbers: ECQUEU750CT-MP - QuEChERS, Mylar packs containing 4 g magnesium sulfate, 1 g sodium chloride, 0.5 g sodium citrate dibasic

More information

SIMULTANEOUS DETERMINATION OF NALTREXONE AND 6- -NALTREXOL IN SERUM BY HPLC

SIMULTANEOUS DETERMINATION OF NALTREXONE AND 6- -NALTREXOL IN SERUM BY HPLC SIMULTANEOUS DETERMINATION OF NALTREXONE AND 6- -NALTREXOL IN SERUM BY HPLC Katja SÄRKKÄ, Kari ARINIEMI, Pirjo LILLSUNDE Laboratory of Substance Abuse, National Public Health Institute Manerheimintie,

More information

STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF AZILSARTAN MEDOXOMIL AND CHLORTHALIDONE IN SOLID DOSAGE FORMS

STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF AZILSARTAN MEDOXOMIL AND CHLORTHALIDONE IN SOLID DOSAGE FORMS Innovare Academic Sciences International Journal of Pharmacy and Pharmaceutical Sciences ISSN- 0975-1491 Vol 6, Issue 6, 2014 Original Article STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION

More information

Analysis of the Vitamin B Complex in Infant Formula Samples by LC-MS/MS

Analysis of the Vitamin B Complex in Infant Formula Samples by LC-MS/MS Analysis of the Vitamin B Complex in Infant Formula Samples by LC-MS/MS Stephen Lock 1 and Matthew Noestheden 2 1 AB SCIEX Warrington, Cheshire (UK), 2 AB SCIEX Concord, Ontario (Canada) Overview A rapid,

More information

International Journal of Research and Reviews in Pharmacy and Applied science. www.ijrrpas.com

International Journal of Research and Reviews in Pharmacy and Applied science. www.ijrrpas.com International Journal of Research and Reviews in Pharmacy and Applied science www.ijrrpas.com P.V.V.Satyanarayana*, Alavala Siva Madhavi NEW SPECTROPHOTOMETRIC METHODS FOR THE QUANTITATIVE ESTIMATION OF

More information

Thermo Scientific SOLAµ SPE Plates Technical Guide. Consistent excellence. for bioanalysis

Thermo Scientific SOLAµ SPE Plates Technical Guide. Consistent excellence. for bioanalysis Thermo Scientific SOLAµ SPE Plates Technical Guide Consistent excellence for bioanalysis SOLAµ - delivering reproducible low volume extractions. Everytime! Thermo Scientific SOLAµ plates are designed for

More information

Implementing New USP Chapters for Analytical Method Validation

Implementing New USP Chapters for Analytical Method Validation Implementing New USP Chapters for Analytical Method Validation March 2010 Ludwig Huber Fax.: +49 7243 602 501 E-mail: Ludwig_Huber@labcompliance.com Today s Agenda Handling Method Changes vs. Adjustments

More information

EUROPEAN COMMISSION DIRECTORATE-GENERAL TAXATION AND CUSTOMS UNION TAX POLICY Excise duties and transport, environment and energy taxes

EUROPEAN COMMISSION DIRECTORATE-GENERAL TAXATION AND CUSTOMS UNION TAX POLICY Excise duties and transport, environment and energy taxes EUROPEAN COMMISSION DIRECTORATE-GENERAL TAXATION AND CUSTOMS UNION TAX POLICY Excise duties and transport, environment and energy taxes Brussels, 18th May 2005 CED No 494 rev 2 Final TAXUD/3711/2004 POETRY:

More information

Stability-indicating High Performance Thin Layer Chromatographic Determination of Clozapine in Tablet Dosage Form

Stability-indicating High Performance Thin Layer Chromatographic Determination of Clozapine in Tablet Dosage Form Stability-indicating High Performance Thin Layer Chromatographic Determination of Clozapine in Tablet Dosage Form Zahid Zaheer *, Mazhar Farooqui 1, S.R.Dhaneshwar 2 *Y.B.Chavan College of Pharmacy, Dr.

More information

Thermo Scientific SOLA SPE cartridges and plates Technical Guide. Join the revolution. unparalleled performance

Thermo Scientific SOLA SPE cartridges and plates Technical Guide. Join the revolution. unparalleled performance Thermo Scientific SOLA SPE cartridges and plates Technical Guide Join the revolution unparalleled performance Join the revolution next-generation SPE Thermo Scientific SOLA products revolutionize Solid

More information

Sensitive and Rapid Determination of Polycyclic Aromatic Hydrocarbons in Tap Water

Sensitive and Rapid Determination of Polycyclic Aromatic Hydrocarbons in Tap Water Sensitive and Rapid Determination of Polycyclic Aromatic Hydrocarbons in Tap Water Chen Jing, 1 Dai Zhenyu, 1 Xu Qun, 1 Liang Lina, 1 and Jeffrey Rohrer 2 1 Thermo Fisher Scientific, Shanghai, People s

More information

High sensitivity assays using online SPE-LC-MS/MS -How low can you go? Mohammed Abrar Unilabs York Bioanalytical solutions, York, UK

High sensitivity assays using online SPE-LC-MS/MS -How low can you go? Mohammed Abrar Unilabs York Bioanalytical solutions, York, UK High sensitivity assays using online SPE-LC-MS/MS -How low can you go? Mohammed Abrar Unilabs York Bioanalytical solutions, York, UK Background Unilabs YBS are a bioanalytical CRO based in York (Uk) Copenhagen

More information

CORESTA RECOMMENDED METHOD Nº 80

CORESTA RECOMMENDED METHOD Nº 80 CORESTA RECOMMENDED METHOD Nº 80 USE OF THE PART-FILTER METHOD FOR THE ESTIMATION OF SMOKERS EXPOSURE TO NICOTINE AND NICOTINE-FREE DRY PARTICULATE MATTER (January 2016) 0. INTRODUCTION The CORESTA Smoking

More information

Oasis HLB Cartridges and 96-Well Plates

Oasis HLB Cartridges and 96-Well Plates CONTENTS I. INTRODUCTION II. SAMPLE PRE-TREATMENT a. Biological Samples b. Solid Samples: Soil, Whole Foods, Tissue c. Aqueous Samples: Water, Beverages d. Non-Aqueous Liquid III. SOLID PHASE EXTRACTION

More information

Analytical Methods for Cleaning Validation

Analytical Methods for Cleaning Validation Available online at www.scholarsresearchlibrary.com Scholars Research Library Der Pharmacia Lettre, 2011, 3 (6): 232-239 (http://scholarsresearchlibrary.com/archive.html) ISSN 0975-5071 USA CODEN: DPLEB4

More information

Thermo Scientific Dionex Chromeleon 7 Chromatography Data System Software

Thermo Scientific Dionex Chromeleon 7 Chromatography Data System Software Thermo Scientific Dionex Chromeleon 7 Chromatography Data System Software Frank Tontala, Thermo Fisher Scientific, Germering, Germany Technical Note 708 Key Words Chromeleon Chromatography Data System,

More information

Extraction of Epinephrine, Norepinephrine and Dopamine from Human Plasma Using EVOLUTE EXPRESS WCX Prior to LC-MS/MS Analysis

Extraction of Epinephrine, Norepinephrine and Dopamine from Human Plasma Using EVOLUTE EXPRESS WCX Prior to LC-MS/MS Analysis Application Note AN844 Extraction of, and from Human Plasma Using EVOLUTE EXPRESS WCX Page 1 Extraction of, and from Human Plasma Using EVOLUTE EXPRESS WCX Prior to LC-MS/MS Analysis Introduction Catecholamines

More information

Determination of Haloacetic Acids and Dalapon in Drinking Water by SPE and GC/ECD*

Determination of Haloacetic Acids and Dalapon in Drinking Water by SPE and GC/ECD* Method 552.1 Revision 1.0 Determination of Haloacetic Acids and Dalapon in Drinking Water by SPE and GC/ECD* UCT Products: EUQAX156 (quaternary amine with Cl - counter ion, 6 ml cartridge)** CLTTP050 (CLEAN-THRU

More information

Center for Drug Evaluation and Research (CDER) Reviewer Guidance' Validation of Chromatographic Methods. November 1994 CMC 3

Center for Drug Evaluation and Research (CDER) Reviewer Guidance' Validation of Chromatographic Methods. November 1994 CMC 3 Center for Drug Evaluation and Research (CDER) Reviewer Guidance' Validation of Chromatographic Methods November 1994 CMC 3 TABLE OF CONTENTS I. INTRODUCTION... 1 II. TYPES OF CHROMATOGRAPHY... 2 A. High

More information

Technical Procedure for the Solid Phase Extraction of Acidic, Neutral and Basic Drugs for GC-MS Analysis

Technical Procedure for the Solid Phase Extraction of Acidic, Neutral and Basic Drugs for GC-MS Analysis Technical Procedure for the Solid Phase Extraction of Acidic, Neutral and Basic Drugs for GC-MS Analysis 1.0 Purpose - This procedure specifies the required elements for the solid phase extraction of acidic,

More information

LACHAT METHOD NUMBER 10-204-00-5-D Rev 1, 21 March 2011 SCOPE AND APPLICATION Approximately 3-500 g CN/L 2-500 g CN/L. 09e

LACHAT METHOD NUMBER 10-204-00-5-D Rev 1, 21 March 2011 SCOPE AND APPLICATION Approximately 3-500 g CN/L 2-500 g CN/L. 09e 1 SIDE BY SIDE COMPARISON TABLE FOR THE DETERMINATION OF CYANIDE BY UV DIGESTION AND AMPEROMETRIC DETECTION FIA METHOD - 10-204-00-5-D (ASTM D7511-09 e ) TOPIC Method ASTM D7511-09e LACHAT METHOD NUMBER

More information

International GMP Requirements for Quality Control Laboratories and Recomendations for Implementation

International GMP Requirements for Quality Control Laboratories and Recomendations for Implementation International GMP Requirements for Quality Control Laboratories and Recomendations for Implementation Ludwig Huber, Ph.D. ludwig_huber@labcompliance.com Overview GMP requirements for Quality Control laboratories

More information

STABILITY TESTING: PHOTOSTABILITY TESTING OF NEW DRUG SUBSTANCES AND PRODUCTS

STABILITY TESTING: PHOTOSTABILITY TESTING OF NEW DRUG SUBSTANCES AND PRODUCTS INTERNATIONAL CONFERENCE ON HARMONISATION OF TECHNICAL REQUIREMENTS FOR REGISTRATION OF PHARMACEUTICALS FOR HUMAN USE ICH HARMONISED TRIPARTITE GUIDELINE STABILITY TESTING: PHOTOSTABILITY TESTING OF NEW

More information

Determination of Anabolic Steroids in Horse Urine by SPE and LC-MS/MS

Determination of Anabolic Steroids in Horse Urine by SPE and LC-MS/MS Summary: Determination of Anabolic Steroids in Horse Urine by SPE and LC-MS/MS UCT Part Numbers: CUNAX226 - Clean-Up C8+NAX, 2mg/6mL BETA-GLUC- ml Beta-Glucuronidase Enzyme, liquid form SLAQ1ID21-3UM -

More information

High performance thin layer chromatographic method for estimation of deflazacort in tablet

High performance thin layer chromatographic method for estimation of deflazacort in tablet ISSN: 2231-3354 Received on: 07-09-2011 Revised on: 11-09-2011 Accepted on: 13-09-2011 High performance thin layer chromatographic method for estimation of deflazacort in tablet Patel Satish A and Patel

More information

Vitamin C quantification using reversed-phase ion-pairing HPLC

Vitamin C quantification using reversed-phase ion-pairing HPLC Vitamin C quantification using reversed-phase ion-pairing HPLC Thomas Grindberg and Kristy Williams Department of Chemistry, Concordia College, 901 8 th St S, Moorhead, MN 56562 Abstract Vitamin C, an

More information

BRIEFING 661.2 Plastic Packaging Systems for Pharmaceutical Use.

BRIEFING 661.2 Plastic Packaging Systems for Pharmaceutical Use. BRIEFING 661.2 Plastic Packaging Systems for Pharmaceutical Use. USP proposes the revision and development of a suite of plastic packaging system standards in the current issue of PF. General test chapter

More information

The Use of Micro Flow LC Coupled to MS/MS in Veterinary Drug Residue Analysis

The Use of Micro Flow LC Coupled to MS/MS in Veterinary Drug Residue Analysis The Use of Micro Flow LC Coupled to MS/MS in Veterinary Drug Residue Analysis Stephen Lock AB SCIEX Warrington (UK) Overview A rapid, robust, sensitive and specific LC-MS/MS method has been developed for

More information

SPIKE RECOVERY AND DETERMINING A METHOD DETECTION LIMIT Pamela Doolittle, University of Wisconsin Madison, pssemrad@wisc.edu 2014

SPIKE RECOVERY AND DETERMINING A METHOD DETECTION LIMIT Pamela Doolittle, University of Wisconsin Madison, pssemrad@wisc.edu 2014 SPIKE RECOVERY AND DETERMINING A METHOD DETECTION LIMIT Pamela Doolittle, University of Wisconsin Madison, pssemrad@wisc.edu 2014 This experiment explores quality assurance practices which are commonly

More information

INTERNATIONAL OLIVE COUNCIL

INTERNATIONAL OLIVE COUNCIL INTERNATIONAL OLIVE COUNCIL COI/T.20/Doc. No 19/Rev. 3 February 2015 ENGLISH Original: ENGLISH Príncipe de Vergara, 154 28002 Madrid España Telef.: +34 915 903 638 Fax: +34 915 631 263 - e-mail: iooc@internationaloliveoil.org

More information

Journal of Chemical and Pharmaceutical Research, 2012, 4(7):3483-3488. Research Article

Journal of Chemical and Pharmaceutical Research, 2012, 4(7):3483-3488. Research Article Available online www.jocpr.com Journal of Chemical and Pharmaceutical Research, 2012, 4(7):3483-3488 Research Article ISSN : 0975-7384 CODEN(USA) : JCPRC5 Simultaneous UV spectrphotometric estimation of

More information

HEXANES. Insoluble in water, soluble in ether, alcohol, and acetone. Neutral to methyl orange (ph indicator) Not more than 0.

HEXANES. Insoluble in water, soluble in ether, alcohol, and acetone. Neutral to methyl orange (ph indicator) Not more than 0. HEXANES Prepared at the 51st JECFA (1998), published in FNP 52 Add 6 (1998) superseding specifications prepared at the 14th JECFA (1970), published in NMRS 48B (1971) and in FNP 52 (1992). ADI "limited

More information

Protocol: HPLC (amino acids)

Protocol: HPLC (amino acids) Page 1 of 6 1. Chemicals Composition M MW gram volume (ml) product code 0-pthaldialdehyde C 8H 6O 2 134.13 Sigma P0657 Perchloric acid HClO 4 3.5 100.46 Dilute 70% stock solution 1:1 with demi to obtain

More information

IN VITRO BINDING BIOEQUIVALENCE STUDY SUMMARY TABLES AND SAS TRANSPORT FORMATTED TABLES FOR DATASET SUBMISSION

IN VITRO BINDING BIOEQUIVALENCE STUDY SUMMARY TABLES AND SAS TRANSPORT FORMATTED TABLES FOR DATASET SUBMISSION IN VITRO BINDING BIOEQUIVALENCE STUDY SUMMARY TABLES AND SAS TRANSPORT FORMATTED TABLES FOR DATASET SUBMISSION I. For Calcium Acetate Drug Products Table I.1 Submission Summary * Drug Product Name Strength(s)

More information

THE ROLE OF RELATIVE RESPONSE FACTOR IN RELATED SUBSTANCES METHOD DEVELOPMENT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

THE ROLE OF RELATIVE RESPONSE FACTOR IN RELATED SUBSTANCES METHOD DEVELOPMENT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC) http://www.rasayanjournal.com Vol.4, No.4 (2011), 919-943 ISSN: 0974-1496 CODEN: RJCABP THE ROLE OF RELATIVE RESPONSE FACTOR IN RELATED SUBSTANCES METHOD DEVELOPMENT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

More information

Determination of Caffeine in Beverages HPLC-1

Determination of Caffeine in Beverages HPLC-1 Determination of in s HPLC-1 Introduction This experiment provides an introduction to the application of High Performance Liquid Chromatography (HPLC) to the solution of complex analytical problems. Cola

More information

Photolytic-Thermal Degradation Study And Method Development Of Rivaroxaban By RP-HPLC

Photolytic-Thermal Degradation Study And Method Development Of Rivaroxaban By RP-HPLC International Journal of PharmTech Research CODEN (USA): IJPRIF ISSN : 0974-4304 Vol.5, No.3, pp 1254-1263, July-Sept 2013 Photolytic-Thermal Degradation Study And Method Development Of Rivaroxaban By

More information

OLIVÉR BÁNHIDI 1. Introduction

OLIVÉR BÁNHIDI 1. Introduction Materials Science and Engineering, Volume 39, No. 1 (2014), pp. 5 13. DETERMINATION OF THE ANTIMONY- AND STRONTIUM- CONTENT OF ALUMINIUM ALLOYS BY INDUCTIVELY COUPLED PLASMA ATOM EMISSION SPECTROMETRY

More information

ANALYSIS OF FOOD AND NATURAL PRODUCTS LABORATORY EXERCISE

ANALYSIS OF FOOD AND NATURAL PRODUCTS LABORATORY EXERCISE ANALYSIS OF FOOD AND NATURAL PRODUCTS LABORATORY EXERCISE Determination of carbohydrates in foodstuff (LC/RID method) Exercise guarantor: Assoc. Prof. Karel Cejpek, Ph.D. CONTENT Required knowledge...

More information

LIQUID CHROMATOGRAPHY HOW MUCH ASPIRIN, ACETAMINOPHEN, AND CAFFEINE ARE IN YOUR PAIN RELIEVER? USING HPLC TO QUANTITATE SUBSTANCES (Revised: 1-13-93)

LIQUID CHROMATOGRAPHY HOW MUCH ASPIRIN, ACETAMINOPHEN, AND CAFFEINE ARE IN YOUR PAIN RELIEVER? USING HPLC TO QUANTITATE SUBSTANCES (Revised: 1-13-93) INTRODUCTION HOW MUCH ASPIRIN, ACETAMINOPHEN, AND CAFFEINE ARE IN YOUR PAIN RELIEVER? USING HPLC TO QUANTITATE SUBSTANCES (Revised: 1-13-93) Headache, sore muscles, arthritis pain... How do you spell relief?

More information

ß-CYCLODEXTRIN SYNONYMS

ß-CYCLODEXTRIN SYNONYMS ß-CYCLODEXTRIN Prepared at the 44th JECFA (1995), published in FNP 52 Add 3 (1995) superseding specifications prepared at the 41st JECFA (1993), published in FNP 52 Add 2 (1993). Metals and arsenic specifications

More information

UV-VIS SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF GABAPENTIN AND METHYLCOBALAMIN IN BULK AND TABLET

UV-VIS SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF GABAPENTIN AND METHYLCOBALAMIN IN BULK AND TABLET International Journal of ChemTech Research CODEN( USA): IJCRGG ISSN : 0974-4290 Vol.2, No.1, pp 695-699, Jan-Mar 2010 UV-VIS SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF GABAPENTIN AND METHYLCOBALAMIN IN

More information

United States Department of Agriculture Food Safety and Inspection Service, Office of Public Health Science

United States Department of Agriculture Food Safety and Inspection Service, Office of Public Health Science CLG-MG/CV2.00 Page 1 of 15 Contents A. INTRODUCTION... 2 B. EQUIPMENT... 3 C. REAGENTS AND SOLUTIONS... 4 D. STANDARDS... 5 E. SAMPLE PREPARATION... 6 F. ANALYTICAL PROCEDURE... 6 G. CONFIRMATION... 8

More information

Standard Analytical Methods of Bioactive Metabolitesfrom Lonicera japonica Flower Buds by HPLC-DAD and HPLC-MS/MS

Standard Analytical Methods of Bioactive Metabolitesfrom Lonicera japonica Flower Buds by HPLC-DAD and HPLC-MS/MS Standard Analytical Methods of Bioactive Metabolitesfrom Lonicera japonica Flower Buds by HPLCDAD and HPLCMS/MS Jongheon Shin College of Pharmacy Seoul National University Summary The standard analytical

More information

By T.Sudha, T.Raghupathi

By T.Sudha, T.Raghupathi Global Journal of Medical research Volume 11 Issue 2 Version 1.0 Type: Double Blind Peer Reviewed International Research Journal Publisher: Global Journals Inc. (USA) Online ISSN: 0975-5888 Reverse Phase

More information

Estimation and Stress Study of a Potent Anticoagulant Drug Rivaroxaban by a Validated HPLC Method

Estimation and Stress Study of a Potent Anticoagulant Drug Rivaroxaban by a Validated HPLC Method 2 ESTIMATION AND STRESS STUDY OF A POTENT ANTICOAGULANT DRUG RIVAROXABAN BY A VALIDATED HPLC METHOD II Estimation and Stress Study of a Potent Anticoagulant Drug Rivaroxaban by a Validated HPLC Method

More information

HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR DETERMINATION OF TADALAFIL IN TABLET DOSAGE FORM

HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR DETERMINATION OF TADALAFIL IN TABLET DOSAGE FORM Volume 1, Issue 3, 2011. ISSN: 2249-3387 Journal home page: http://www.ajptr.com/ HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR DETERMINATION OF TADALAFIL IN TABLET DOSAGE FORM Satish A. Patel

More information