Analysis of Organophosphorus Pesticides in Milk Using SPME and GC-MS/MS. No. GCMS No. SSI-GCMS Shilpi Chopra, Ph.D.
|
|
- Derrick Stevens
- 8 years ago
- Views:
Transcription
1 Gas Chromatograph Mass Spectrometer No. GCMS-1603 Analysis of Organophosphorus Pesticides in Milk Using SPME and GC-MS/MS Shilpi Chopra, Ph.D. Introduction Organophosphorus (OP) pesticides are a class of insecticides known for their acute toxicity towards a large variety of insects, and a relatively lower persistence in the environment compared to organochlorine pesticides. Therefore, the OP class of pesticides are more commonly used on food crops, despite the higher toxicity they present towards mammals. These compounds inhibit acetylcholinesterase enzymes in the central nervous system, eventually causing paralysis. Exposure in humans occurs through ingestion of contaminated food products, thus it is important to develop analytical techniques for complex food matrices to ensure safe consumption levels for OP pesticides are maintained. Gas chromatography mass spectrometry (GC/MS) instrumentation is a powerful tool for the separation and identification of volatile and semi-volatile compounds, including many OP pesticides. Gas chromatography coupled to a triple quadrupole mass spectrometer (GC-MS/MS) allows for even greater separation, as the mass spectrometer is operated in the Multiple Reaction Monitoring (MRM) mode with two stages of mass analysis. When using MRM mode, the sample is ionized at the ion source and a single, high-mass high-intensity ion is selected in the first quadrupole (Q1); this fragment is referred to as a precursor ion. The precursor ion is focused toward the second quadrupole, also called the Collision Cell, where it collides with an inert gas (argon) and is fragmented to produce product ions. A single product ion is selected using the third quadrupole (Q3) and detected by the electron multiplier. This mode of detection virtually eliminates background interference, making GC-MS/MS a powerful technique with improved sensitivity, selectivity, and specificity. interfering matrices. Detection and quantitation of pesticides in food products fit these criteria, and complimentary sample preparation techniques are needed to simplify the analyses to increase sample throughput through automation. Solid Phase Micro- Extraction (SPME) has produced promising results when used as a sample preparation technique for complex matrices. In the SPME process, a fused silica fiber treated with a compound-specific coating is either exposed to the equilibrated sample headspace, or directly immersed into the sample. The analytes are then absorbed or adsorbed onto the fiber, and subsequently thermally desorbed from the fiber in the GC inlet. SPME involves various parameters, such as incubation temperature and time, desorption time and temperature, and extraction time and temperature. If not properly optimized, these can affect detection levels, which is why a statistical tool is needed to evaluate these parameters. The SPME technique has several desirable advantages; most importantly it does not require the use of harmful organic solvents, and it is easily automated. This application note describes development of a fully automated SPME extraction method combined with GC-MS/MS analysis for detection and quantitation of OP pesticides in a complex milk matrix. The Shimadzu GCMS-TQ8040 triple quadrupole mass spectrometer used for this application note is shown in Figure 1. The SPME method development and validation were fully automated using the Shimadzu AOC-6000 Multifunctional Autosampler. GC-MS/MS analytical instruments are widely used in applications requiring detection of specific target compounds at low concentrations in complex, Figure 1: Shimadzu GCMS-TQ8040 Used for Detection and Quantitation of OP Pesticides
2 Experimental Sample Preparation Standard solutions of eight individual OP pesticides (demeton-s-methyl, sulfotep, disulfoton, methyl parathion, dichlorvos, fenitrothion, chlorpyrifos, and ethion) were acquired from Absolute Standard, Inc. (Hamden, USA). A stock working solution was prepared with each pesticide at 100 µg/ml (partsper-million, ppm). Milk was purchased from a local grocery store, and spiked with the working solution to 1.25 µg/ml for method development. Lower concentrations, in the ng/ml (parts-per-billion, ppb) range were used for calibration and method validation. Headspace - Solid Phase Micro Extraction (HS-SPME) The HS-SPME extraction was performed using a fiber coated with polydimethylsiloxane-divinylbenzene (PDMS-DVB, 65 μm) (Supelco, Bellefonte, USA). Individual aliquots of milk were placed in 20-mL SPME vials and spiked with the OP pesticide mix to yield a constant concentration of 1.25 µg/ml. To minimize the number of individual analyses required, a half factorial experimental design was used to optimize the experimental variables affecting the SPME extraction. The half-factorial experimental design provides the maximum amount of information with the least number of analyses. It can be used to determine the effect from each independent parameter, and to identify any interaction effects when more than one parameter influences the observed result. Five SPME parameters were optimized: sample volume, desorption time, incubation temperature, incubation time (sample equilibration time prior to introducing the SPME fiber), and extraction time (exposure of the SPME fiber to the sample). Two test values were established for each parameter, one at the high end of the range (H) and one at the low end (L), as shown in Table 1. This type of two-level experimental design is called half fraction factorial design, or factorial design, and is a common technique because it provides the greatest amount of information with the fewest number of instrument analyses. It also will provides information required to advance to a multi-level response surface experiment if necessary. Blanks were run between samples to verify that there was no carry over. Addition of a salt was not tested because adequate detection levels were achieved without the salt. Table 1: Half Factorial Experimental Design for SPME Method Optimization using PDMS-DVB Fiber Sample Volume (ml) Desorption Time (min) Incubation Temperature ( C) Incubation Time (min) Extraction Time (min) High Parameter (H) Low Parameter (L) Run # X1 Sample Volume X2 Desorption Time X3 Incubation Temperature X4 Incubation Time 1 H H H H H 2 H H H L L 3 H H L L H 4 H L L L L 5 L L L L H 6 H L H H L 7 H L L H H 8 H H L H L 9 L L L H L 10 L L H H H 11 L H H H L 12 H L H L H 13 L H L H H 14 L L H L L 15 L H L L L 16 L H H L H X5 Extraction Time
3 GC-MS/MS The analyses were performed on a Shimadzu GCMS- TQ8040. Analytes were desorbed from the SPME fiber with inlet temperature of 250 C and using a splitless injection. Chromatographic separation was achieved using a capillary column (SH-Rxi-5HT Column; 30 m 0.25 mm ID 0.25 μm film) with helium carrier gas and a flow rate of 1.44 ml/minute. The oven temperature was programmed, with an initial temperature of 80 C for 3 minutes and a temperature ramp of 15 C/minute to 280 C, followed by a 2 minute hold. The GC-MS/MS was operated in the Multiple Reaction Monitoring (MRM) mode. Three transitions were monitored for each target compound, one for quantitation, and two additional transitions for confirmation. The Shimadzu Smart Pesticide Database was used as the foundation for creating the MRM analysis method. The Smart Pesticide Database includes up to six fully optimized MRM transitions and collision energies (CEs) for 479 pesticides and Retention Indices (RI) for accurately predicting compound retention times. The ion source was kept at 200 C, with an interface temperature of 260 C and solvent delay time of 3 minutes. The GC- MS/MS parameters are summarized in Table 2. Table 2: Optimized GC-MS/MS Operating Parameters GC-MS/MS Parameter Optimized Value Inlet Temperature 250 C Constant Linear Velocity Mode Column Flow 1.44 ml/minute Injection Mode Splitless Oven temperature Program 80 C (3 minutes) 15 C/minute to 280 C (2 minutes) Interface Temperature 260 C Ion Source Temperature 200 C MS/MS Mode MRM Results and Discussion GC-MS/MS The MRM method was established by using the three most prominent MRM transitions for the OP pesticides found in the Smart Database; compound retention times were predicted for the method using the principle of Retention Indices. Figure 2 shows an MRM chromatogram of the 8-pesticide mix at 10 µg/ml, with all peaks baseline resolved. Figure 2: MRM Chromatogram of the Eight OP Pesticides at 10 µg/ml
4 HS-SPME Method Development The results obtained from the evaluation of the significant parameters by half factorial design are summarized in the Pareto Chart of Standardized Effects, shown in Figure 3. The Pareto chart for each OP Pesticide shows the influence that the most significant of the five test parameters had on the instrument response for that specific compound, as well as any possible cross, or interactive effects among these parameters. Pareto charts illustrate the magnitude and the importance of any individual parameter, or combination of parameters, on the instrument response. Parameters with significant effects are labeled A, B, and C, along the Y-axis, with the length of the bar along the X-axis illustrating the relative magnitude of that effect. Where a combination of two or more parameters is determined to have a significant effect, it is included and labeled AB, AC, BC, etc. The horizontal bar for each parameter represents the normalized, or relative value of that effect. A vertical reference line on the chart indicates that any parameter which extends beyond this value is potentially important for the optimization of the instrumental method. Figure 3: Pareto Chart of Standardized Effects for 8 OP Pesticides Extracted by HS-SPME
5 As can be seen by the Pareto charts in Figure 3, only two of the five test variables were found to consistently have a significant effect on extraction of the pesticides during the SPME method development, as indicated by extension of the bar beyond the vertical red line. The Incubation Temperature (parameter A) crosses the vertical red reference line for seven of the eight pesticides, indicating that it was a decisive factor for HS-SPME extraction experiment. This is in agreement with HS- SPME principle, as the incubation temperature is a key factor for driving pesticides from sample into the headspace during the equilibration step. Extraction Time (parameter B) was significant for 6 of the 8 pesticides, indicating that it was also an important factor for SPME extraction of pesticides from the milk. The remaining 3 parameters, Incubation Time, Sample Volume, and Desorption Time, were found to have little or no effect on the final results using this approach. The optimized HS- SPME parameters are shown in Table 3. Table 3: Optimized HS-SPME Parameters SPME Parameter Incubation Temperature Incubation Time Extraction Time Desorption Time Sample Volume In addition to the Pareto charts, a three-dimensional surface plot of the factors can provide additional information. A surface plot displays a threedimensional view that provides a clear picture of the relationship between two variables. If the regression model contains only the main effect and no interaction effect, the fitted response will be flat plane. If the model contains interaction effects, it will be a curved surface. The response surface graph obtained from the results of the fractional factorial design for the OP pesticides revealed that there is a relationship between the Incubation Temperature (A) and Extraction Time (B). This effect is seen on the Pareto Charts by the bar labeled AB extending beyond the vertical line for six of the eight pesticides, and is further illustrated in the example of Dichlovos shown in Figure 4. The x- and y-axes are Incubation Temperature (A) and Extraction Time (B), respectively, and the z-axis is compound response measured as peak area. Optimized Value 100 o C 10 minutes 60 minutes 3 minutes 8 ml Figure 4: Response Surface of Diclovos
6 Method Validation Calibration standards were prepared and analyzed using the optimized HS-SPME and GC-MS/MS parameters, with concentrations ranging from 20 to 1000 µg/l (ppb). Figure 5 shows the individual calibrations curves for all 8 pesticides, with the corresponding correlation coefficients illustrating linearity. Figure 5: Calibration Plots for all 8 Pesticides in Milk using HS-SPME and GC-MS/MS
7 Of the eight OP pesticides analyzed, seven were linear across the calibration range with correlation coefficients above 0.99, while one compound, demeton-s-methyl, displayed linearity only from µg/l using this method. There are two possible reasons for the non-linear response of demeton-smethyl. First, while optimizing the SPME method, it was observed that the peak area for demeton-smethyl increased considerably at low extraction temperatures, and presented comparatively lower peak areas at the higher temperatures. Using a liquid syringe injection technique for comparison, there were no unexpected peaks in the chromatogram. However, when using the HS-SPME extraction technique, an additional peak was seen at minutes, which is most likely a degradation product of the target analyte caused by the higher temperatures. (Figure 6.) The second, less likely possibility could be attributed to the chemistry of the fiber. As PDMS-DVB operates on an adsorption mechanism, competition for adsorption sites may explain the loss of response for Demeton-S-methyl Figure 6: Comparison of MRM Chromatograms of Demeton-S-methyl Analyzed using Liquid Syringe Injection (6a) and HS-SPME (6b) Table 4 lists the method validation statistics as defined by IUPAC guidelines, which include linearity, repeatability as % RSD, and accuracy as % Recovery for extraction of pesticides in milk by the HS-SPME method developed here. All pesticides had repeatability of less than 12.8 %, and recovery between 82 and 105 %, as calculated using a spiking level of 20 µg/l.
8 Table 4: Method Validation Statistics Pesticide Conc. in µg/l (R 2 ) % RSD (20 µg/l) % Recovery (20 µg/l) Dicholorovos (0.998) Demeton-S-Methyl (0.993) Sulfotep (0.998) Disulfoton (0.995) Methyl Parathion (0.997) Fenitrothin (0.996) Chlorpyrifos (0.998) Ethion (0.998) Conclusions A method based on HS-SPME, presented here for the analysis of organophosphorus pesticides in milk, was developed using a fully automated AOC-6000 Autosampler. SPME- GC-MS/MS in multiple reaction monitoring (MRM) mode was used for the trace analysis of pesticides in milk. The method was calibrated from 20 µg/l to 1000 µg/l, and all validation statistics were within an acceptable range. This is attributed to effective extraction using automated SPME which ensures precision by eliminating analysis variables in sample preparation and MS-MS which allows monitoring of transitions specific to each pesticide, delivering high selectivity and resulting low noise. References 1. The Smart Forensic Database, Shimadzu Corporation (Japan), is part of the Smart Database Series. The database contains 480 pesticides and approximately 2,680 transitions, and eliminates the need to configure complicated analysis conditions. Retention Indices (RI) are registered for all components, enabling easy updating of retention times via the AART function. Analysis by the internal standard method is also supported, with MRM transitions and RIs registered for compounds commonly used as internal standards for pesticides. 2. Antony,Jiju: Design of Experiments for Engineers and Scientists: Butterworth- Heinemann, Sep 5, 2003, Pages Volante, Marco; Pontello, Mirella: Application of Solid Phase Micro-Extraction (SPME) to the analysis of pesticide residues in vegetables: 56(7); , First Edition: January 2016 SHIMADZU Corporation SHIMADZU SCIENTIFIC INSTRUMENTS 7102 Riverwood Drive, Columbia, MD 21046, USA Phone: / , Fax: URL: For Research Use Only. Not for use in diagnostic procedures. The contents of this publication are provided to you as is without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. Shimadzu Corporation, 2016
Chemistry 321, Experiment 8: Quantitation of caffeine from a beverage using gas chromatography
Chemistry 321, Experiment 8: Quantitation of caffeine from a beverage using gas chromatography INTRODUCTION The analysis of soft drinks for caffeine was able to be performed using UV-Vis. The complex sample
More informationMultifunctional Autosampler AOC-6000 C146-E272A
Multifunctional Autosampler C146-E272A Multifunctional Autosampler Multifunctional Autosampler Dramatically Improves GC/MS Analysis Productivity Automatic Switching Between Three GC/MS Sample Injection
More informationSimultaneous Qualitative and Quantitative Data Acquisition for Research of Diabetes Drugs
Liquid Chromatography Mass Spectrometry SSI-LCMS-068 Simultaneous Qualitative and Quantitative Data Acquisition for Research of Diabetes Drugs LCMS-8050 Summary By utilizing the LCMS-8050 s ultrafast scan
More informationGas Chromatography. Let s begin with an example problem: SPME head space analysis of pesticides in tea and follow-up analysis by high speed GC.
Gas Chromatography Let s begin with an example problem: SPME head space analysis of pesticides in tea and follow-up analysis by high speed GC. Samples in 10mL sealed glass vials were placed in the MPS-2
More informationHow To Test For Contamination In Large Volume Water
Automated Solid Phase Extraction (SPE) of EPA Method 1694 for Pharmaceuticals and Personal Care Products in Large Volume Water Samples Keywords Application Note ENV0212 This collaboration study was performed
More informationTechnical Report. Automatic Identification and Semi-quantitative Analysis of Psychotropic Drugs in Serum Using GC/MS Forensic Toxicological Database
C146-E175A Technical Report Automatic Identification and Semi-quantitative Analysis of Psychotropic Drugs in Serum Using GC/MS Forensic Toxicological Database Hitoshi Tsuchihashi 1 Abstract: A sample consisting
More informationOverview. Triple quadrupole (MS/MS) systems provide in comparison to single quadrupole (MS) systems: Introduction
Advantages of Using Triple Quadrupole over Single Quadrupole Mass Spectrometry to Quantify and Identify the Presence of Pesticides in Water and Soil Samples André Schreiber AB SCIEX Concord, Ontario (Canada)
More informationDetermination of Pesticide Residues in Drinking Water Using Automated Solid-Phase Extraction and Gas Chromatography with Nitrogen Phosphorus Detection
Determination of Pesticide Residues in Drinking Water Using Automated Solid-Phase Extraction and Gas Chromatography with Nitrogen Phosphorus Detection Application Note 1097 Liu Qian, Zheng Hongguo and
More informationACETALDEHYDE 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 informationQuantitative analysis of anabolic steroids in control samples from food-producing animals using a column-switching LC-HESI-MS/MS assay
PO-CON1484E Quantitative analysis of anabolic steroids in control samples from food-producing animals using a column-switching ASMS 014 TP85 David R. Baker 1, John Warrander 1, Neil Loftus 1, Simon Hird
More information# LCMS-35 esquire series. Application of LC/APCI Ion Trap Tandem Mass Spectrometry for the Multiresidue Analysis of Pesticides in Water
Application Notes # LCMS-35 esquire series Application of LC/APCI Ion Trap Tandem Mass Spectrometry for the Multiresidue Analysis of Pesticides in Water An LC-APCI-MS/MS method using an ion trap system
More informationStep-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 informationEnhancing GCMS analysis of trace compounds using a new dynamic baseline compensation algorithm to reduce background interference
Enhancing GCMS analysis of trace compounds using a new dynamic baseline compensation algorithm to reduce background interference Abstract The advantages of mass spectrometry (MS) in combination with gas
More information1.1 This test method covers the qualitative and quantitative determination of the content of benzene and toluene in hydrocarbon wax.
Standard Method for Analysis of Benzene and Toluene Content in Hydrocarbon Waxes by Headspace Gas Chromatography EWF METHOD 002/03 (Version 1 Reviewed 2015) 1 Scope 1.1 This test method covers the qualitative
More informationAppNote 6/2003. Analysis of Flavors using a Mass Spectral Based Chemical Sensor KEYWORDS ABSTRACT
AppNote 6/2003 Analysis of Flavors using a Mass Spectral Based Chemical Sensor Vanessa R. Kinton Gerstel, Inc., 701 Digital Drive, Suite J, Linthicum, MD 21090, USA Kevin L. Goodner USDA, Citrus & Subtropical
More informationAnalysis 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 informationMultiQuant Software Version 3.0 for Accurate Quantification of Clinical Research and Forensic Samples
MultiQuant Software Version 3.0 for Accurate Quantification of Clinical Research and Forensic Samples Fast and Efficient Data Review, with Automatic Flagging of Outlier Results Adrian M. Taylor and Michael
More informationFipronil Analysis By GC/XSD following Post-Extraction Gel Permeation Chromatography Cleanup
Application Note 25570306 Fipronil Analysis By GC/XSD following Post-Extraction Gel Permeation Chromatography Cleanup Keywords Gel Permeation Chromatography GPC AutoPrep 2000 Pesticides RapidVap N2 System
More informationMEPS - Micro Extraction by Packed Sorbent Online SPE for GC and LC sample preparation - Extraction to injection in a single process
- Micro Extraction by Packed Sorbent Online SPE for GC and LC sample preparation - Extraction to injection in a single process Save Hours in Sample Preparation Reduce the time to prepare and inject samples
More informationExtraction 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 informationSPE, LC-MS/MS Method for the Determination of Ethinyl Estradiol from Human Plasma
SPE, LC-MS/MS Method for the Determination of Ethinyl Estradiol from uman Plasma Krishna Rao Dara, Dr. Tushar N. Mehta, Asia Pacific Center of Excellence, Thermo Fisher Scientific, Ahmedabad, India Application
More informationIncreasing the Multiplexing of High Resolution Targeted Peptide Quantification Assays
Increasing the Multiplexing of High Resolution Targeted Peptide Quantification Assays Scheduled MRM HR Workflow on the TripleTOF Systems Jenny Albanese, Christie Hunter AB SCIEX, USA Targeted quantitative
More informationEnhancing Utility and Throughput of SPME using Advanced Automation Strategies
Supelco Innovation Seminars November 11 th, 2010 Atlanta, GA Enhancing Utility and Throughput of SPME using Advanced Automation Strategies Presented by Tom Tobien, Ph.D. Analytical Chemist, LEAP Technologies,
More informationSCION SQ Series GC-MS
SCION SQ Series GC-MS The Gas Chromatographers Detector SCION SQ TM GC-MS The SCION SQ series GC-MS systems combine innovative engineering with detailed cutomer requirements to produce a truly innovative
More informationQuantitation of Drugs in Dried Bloodstains. Thomas Meyer Anna Gomenyuk Nadiah Lester
Quantitation of Drugs in Dried Bloodstains Thomas Meyer Anna Gomenyuk Nadiah Lester Objective To find the quantitative value of drugs in dried bloodstains Currently Cloth With Dried Bloodstain Containing
More informationUltra Fast UHPLC-LCMSMS Method Development in Clinical Drug Monitoring
PO-CON1359E Ultra Fast UHPLC-LCMSMS Method Development in HPLC 2013 MASS-09 Anja Grüning 1 ; Brigitte Richrath 1 ; Klaus Bollig 2 ; Sven Vedder 1 ; Robert Ludwig 1 1 Shimadzu Europa GmbH, Duisburg, Germany;
More informationFractional Distillation and Gas Chromatography
Fractional Distillation and Gas Chromatography Background Distillation The previous lab used distillation to separate a mixture of hexane and toluene based on a difference in boiling points. Hexane boils
More informationGuidance 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 informationA VISION to On-Line SPE PTV GC MS Determination of Organic Micro Pollutants in Surface Water
A VISION to On-Line SPE PTV GC MS Determination of Organic Micro Pollutants in Surface Water Sjaak de Koning 1, Mark van Lieshout 2, Hans-Gerd Janssen 2 and Wil van Egmond 1 1 ATAS, De Run 4334, PO Box
More informationExpectations for GC-MS Lab
Expectations for GC-MS Lab Since this is the first year for GC-MS to be used in Dr. Lamp s CHEM 322, the lab experiment is somewhat unstructured. As you move through the two weeks, I expect that you will
More informationThe 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 information6. ANALYTICAL METHODS
45 6.1 BIOLOGICAL MATERIALS No methods were located that are routinely used for the detection of BCEE in biological materials. Norpoth et al. (1986) reported a method for measuring thiodiglycolic acid
More informationA High Throughput Automated Sample Preparation and Analysis Workflow for Comprehensive Forensic Toxicology Screening using LC/MS/MS
A High Throughput Automated Sample Preparation and Analysis Workflow for Comprehensive Forensic Toxicology Screening using LC/MS/MS AB SCIEX QTRAP 4500 LC/MS/MS System and Gerstel, Inc. MultiPurpose Sampler
More informationAnalyzing Small Molecules by EI and GC-MS. July 2014
Analyzing Small Molecules by EI and GC-MS July 2014 Samples Appropriate for GC-MS Volatile and semi-volatile organic compounds Rule of thumb,
More informationAPI 3200 LC/MS/MS SYSTEM. Performance, productivity and value combined
API 3200 LC/MS/MS SYSTEM Performance, productivity and value combined API 3200 LC/MS/MS SYSTEM Reliability, reproducibility, and confidence in your data. With an unmatched heritage of technological innovation
More informationINTEGRATED TECHNOLOGY TO SEE THE WHOLE PICTURE. AxION iqt GC/MS/MS
AxION iqt GC/MS/MS INTEGRATED TECHNOLOGY TO SEE THE WHOLE PICTURE IDENTIFY WHAT YOU RE LOOKING FOR (AND EVEN WHAT YOU RE NOT) The GC/MS/MS Solution for the Work You Do The ideal solution for industrial,
More informationOverview. Introduction. AB SCIEX MPX -2 High Throughput TripleTOF 4600 LC/MS/MS System
Investigating the use of the AB SCIEX TripleTOF 4600 LC/MS/MS System for High Throughput Screening of Synthetic Cannabinoids/Metabolites in Human Urine AB SCIEX MPX -2 High Throughput TripleTOF 4600 LC/MS/MS
More informationPesticide Analysis by Mass Spectrometry
Pesticide Analysis by Mass Spectrometry Purpose: The purpose of this assignment is to introduce concepts of mass spectrometry (MS) as they pertain to the qualitative and quantitative analysis of organochlorine
More informationDetermination 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 informationSIMULTANEOUS 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 informationSimultaneous qualitative and quantitative analysis using the Agilent 6540 Accurate-Mass Q-TOF
Simultaneous qualitative and quantitative analysis using the Agilent 654 Accurate-Mass Q-TOF Technical Overview Authors Pat Perkins Anabel Fandino Lester Taylor Agilent Technologies, Inc. Santa Clara,
More informationAgilent Enhanced Matrix Removal Lipid LOSE THE LIPIDS, FIND YOUR ANALYTES
Agilent Enhanced Matrix Removal Lipid LOSE THE LIPIDS, FIND YOUR ANALYTES AGILENT ENHANCED MATRIX REMOVAL LIPID ARE LIPIDS WEIGHING YOUR SAMPLES DOWN? Interference from lipids is a problem for labs measuring
More informationUtilization of Rapid LC-MS for Screening and Quantitative Analysis of Pesticides in Food Matrix using an Exactive Plus Benchtop Orbitrap Platform
Utilization of Rapid LC-MS for Screening and Quantitative Analysis of Pesticides in Food Matrix using an Exactive Plus Benchtop Orbitrap Platform Charles Yang, Leo Wang, Dipankar Ghosh, Jonathan Beck,
More informationThe Characterization of Perfume Fragrances Using GC/MS, Headspace Trap and Olfactory Port
APPLICATION NOTE Gas Chromatography/ Mass Spectrometry Authors: Andrew Tipler Sheila Eletto PerkinElmer, Inc. Shelton, CT The Characterization of Perfume Fragrances Using GC/MS, Headspace Trap and Olfactory
More informationHow To Analyze Pesticide Levels In Lemon Oil
AppNote 9/2006 Target GC-MS Analysis using Accelerated Column Heating and Interactive Deconvolution Software Albert Robbat Tufts University, Chemistry Department, Medford, MA 02155, USA Andreas Hoffmann
More informationMulti Pesticides Residue analysis in Ayurvedic cough Syrup by GCMS/MS using QuEChERS extraction method
PO-CON679E Multi Pesticides Residue analysis in Ayurvedic cough Syrup by GCMS/MS using QuEChERS extraction method ASMS 206 ThP 47 Durvesh Sawant (), Ankush Bhone (), Dheeraj Handique (), Prashant Hase
More informationDetermination of Polycyclic Aromatic Hydrocarbons (PAH) in Food with GC-MS/MS
Determination of Polycyclic Aromatic Hydrocarbons (PAH) in Food with GC-MS/MS Thorsten Bernsmann, Peter Fürst Chemical and Veterinary Analytical Institute Münsterland-Emscher-Lippe Joseph-König-Str. 40,
More informationMultiQuant Software 2.0 for Targeted Protein / Peptide Quantification
MultiQuant Software 2.0 for Targeted Protein / Peptide Quantification Gold Standard for Quantitative Data Processing Because of the sensitivity, selectivity, speed and throughput at which MRM assays can
More informationSamples RMN070714. Analytical Report (0714-63) GC/FID Analysis (RM01) Nicotine Purity
For the benefit of VaporFi, Inc. Samples RMN070714 Analytical Report (0714-63) GC/FID Analysis (RM01) Nicotine Purity GC/MS Analysis (QG02) Anabasine, Anatabine, Myosmine, Nornicotine Enthalpy Analytical,
More informationAccurate Mass Screening Workflows for the Analysis of Novel Psychoactive Substances
Accurate Mass Screening Workflows for the Analysis of Novel Psychoactive Substances TripleTOF 5600 + LC/MS/MS System with MasterView Software Adrian M. Taylor AB Sciex Concord, Ontario (Canada) Overview
More informationOpiates in Urine by SAMHSA GC/MS
application Note Gas Chromatography/ Mass Spectrometry Author Timothy D. Ruppel PerkinElmer, Inc. Shelton, CT 06484 USA Opiates in Urine by SAMHSA GC/MS Introduction The United States Department of Health
More informationMethod development for analysis of formaldehyde in foodsimulant. melamine-ware by GC-MS and LC-MS/MS. Internal Technical Report
of melamine-ware by GC-MS and LC-MS/MS Page 1 of 15 Method development for analysis of formaldehyde in foodsimulant extracts of melamine-ware by GC-MS and LC-MS/MS December 2012 Contact Point: Chris Hopley
More informationApplication 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 informationA Navigation through the Tracefinder Software Structure and Workflow Options. Frans Schoutsen Pesticide Symposium Prague 27 April 2015
A Navigation through the Tracefinder Software Structure and Workflow Options Frans Schoutsen Pesticide Symposium Prague 27 April 2015 Kings day in The Netherlands 1 Index Introduction Acquisition, Method
More informationS olid Ph ase Extraction (SP E) Method:
Solid Phase Extraction of US EPA 535 for Chloroacetanilide and Acetamide Degradates in Drinking Water Samples Prior to Liquid Chromatography/ Tandem Mass Spectrometry Toni Hofhine, Horizon Technology,
More informationJennifer L. Simeone and Paul D. Rainville Waters Corporation, Milford, MA, USA A P P L I C AT ION B E N E F I T S INT RO DU C T ION
A Validated Liquid-Liquid Extraction Method with Direct Injection of Hexane for Clopidogrel in Human Plasma Using UltraPerformance Convergence Chromatography (UPC 2 ) and Xevo TQ-S Jennifer L. Simeone
More informationApplication of TargetView software within the food industry - the identi cation of pyrazine compounds in potato crisps
Application Note: ANTV10 Application of TargetView software within the food industry - the identi cation of pyrazine compounds in potato crisps Abstract In order to regulate product safety and quality
More informationGC METHODS FOR QUANTITATIVE DETERMINATION OF BENZENE IN GASOLINE
ACTA CHROMATOGRAPHICA, NO. 13, 2003 GC METHODS FOR QUANTITATIVE DETERMINATION OF BENZENE IN GASOLINE A. Pavlova and R. Ivanova Refining and Petrochemistry Institute, Analytical Department, Lukoil-Neftochim-Bourgas
More informationTHERMAL DESORPTION. Introduction and Principles. Focusing on Volatiles
THERMAL DESORPTION Introduction and Principles Thermal Desorption Thermal desorption is a simple extension of the technique of gas chromatography (GC) It involves the use of heat and a flow of inert gas
More informationLC-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 informationEPA Method RSK 175 Dissolved Gasses in Water Matrices using the Teledyne Tekmar HT3 Headspace Analyzer. HT3 Application Note.
EPA Method RSK 175 Dissolved Gasses in Water Matrices using the Teledyne Tekmar HT3 Headspace Analyzer HT3 Application Note Introduction The analysis of dissolved gases in ground water is important in
More informationThe Scheduled MRM Algorithm Enables Intelligent Use of Retention Time During Multiple Reaction Monitoring
The Scheduled MRM Algorithm Enables Intelligent Use of Retention Time During Multiple Reaction Monitoring Delivering up to 2500 MRM Transitions per LC Run Christie Hunter 1, Brigitte Simons 2 1 AB SCIEX,
More informationAppNote 1/2014. Automated Hydrolysis, DPX Extraction and LC/MS/MS Analysis of Pain Management Drugs from Urine KEYWORDS ABSTRACT
AppNote 1/2014 Automated Hydrolysis, DPX Extraction and LC/MS/MS Analysis of Pain Management Drugs from Urine Fred D. Foster, John R. Stuff, Edward A. Pfannkoch GERSTEL, Inc., 701 Digital Dr. Suite J,
More informationSimultaneous Metabolite Identification and Quantitation with UV Data Integration Using LightSight Software Version 2.2
Technical ote Simultaneous Metabolite Identification and Quantitation with UV Data Integration Using LightSight Software Version 2.2 Alek. Dooley, Carmai Seto, esham Ghobarah, and Elliott B. Jones verview:
More informationSimultaneous Quantitation of 43 Drugs in Human Urine with a Dilute-and-Shoot LC-MS/MS Method
Simultaneous Quantitation of 4 Drugs in Human Urine with a Dilute-and-Shoot LC-MS/MS Method Xiang He and Marta Kozak, Thermo Fisher Scientific, San Jose, CA Application Note 76 Key Words TSQ Quantum Access
More informationAppNote 1/2008. Automated Disposable Pipette Extraction of Pesticides from Fruits and Vegetables KEYWORDS ABSTRACT
AppNote 1/2008 Automated Disposable Pipette Extraction of Pesticides from Fruits and Vegetables William E. Brewer, Hongxia Guan, Stephen L. Morgan The University of South Carolina, Columbia, SC, USA Fred
More informationAMD Analysis & Technology AG
AMD Analysis & Technology AG Application Note 120419 Author: Karl-Heinz Maurer APCI-MS Trace Analysis of volatile organic compounds in ambient air A) Introduction Trace analysis of volatile organic compounds
More informationIntroduction. Methods. Sample Processing
PO-CON1656 High-sensitivity, high-throughput quantitation of catecholamines and metanephrine in plasma by automated WCX-SP coupled to LC/MS/MS for clinical research ASMS 2016 MP-080 Ichiro HIRANO 1, Atsuhiko
More informationLC-MS/MS, the new reference method for mycotoxin analysis
LC-MS/MS, the new reference method for mycotoxin analysis What is necessary for the implementation of the multi-residue mycotoxin method in an analytical laboratory? Azel Swemmer azel@fdalab.co.za AFMA
More informationBackground Information
1 Gas Chromatography/Mass Spectroscopy (GC/MS/MS) Background Information Instructions for the Operation of the Varian CP-3800 Gas Chromatograph/ Varian Saturn 2200 GC/MS/MS See the Cary Eclipse Software
More informationUHPLC/MS: An Efficient Tool for Determination of Illicit Drugs
Application Note: 439 UHPLC/MS: An Efficient Tool for Determination of Illicit Drugs Guifeng Jiang, Thermo Fisher Scientific, San Jose, CA, USA Key Words Accela UHPLC System MSQ Plus MS Detector Drugs
More informationMass Spectrometry Signal Calibration for Protein Quantitation
Cambridge Isotope Laboratories, Inc. www.isotope.com Proteomics Mass Spectrometry Signal Calibration for Protein Quantitation Michael J. MacCoss, PhD Associate Professor of Genome Sciences University of
More informationCONFIRMATION 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 informationCRYOCOOLER CONTAMINATION STUDY. S.W.K. Yuan, D.T.Kuo, and A.S. Loc. BEI Technologies, Cryocooler Group Sylmar, CA 91342 ABSTRACT
CRYOCOOLER CONTAMINATION STUDY S.W.K. Yuan, D.T.Kuo, and A.S. Loc EI Technologies, Cryocooler Group Sylmar, CA 91342 ASTRACT Eliminating or reduction of contamination is essential for the success of cryocoolers
More informationVALIDATION 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 informationAlignment and Preprocessing for Data Analysis
Alignment and Preprocessing for Data Analysis Preprocessing tools for chromatography Basics of alignment GC FID (D) data and issues PCA F Ratios GC MS (D) data and issues PCA F Ratios PARAFAC Piecewise
More informationFast, Reproducible LC-MS/MS Analysis of Dextromethorphan and Dextrorphan
Fast, Reproducible LC-MS/MS Analysis of and Kimberly Phipps, Thermo Fisher Scientific, Runcorn, Cheshire, UK Application Note 685 Key Words Accucore C18, dextromethorphan, dextrorphan, SOLA CX Abstract
More informationCliquid Drug Screen & Quant Software for Routine Forensic Toxicology. great interest in forensic, toxicological and clinical research laboratories.
Application Note Cliquid Drug Screen & Quant Software A Fast and Sensitive LC/MS/MS Method for the Quantitation and Confirmation of 30 Benzodiazepines and Nonbenzodiazepine Hypnotics in Forensic Urine
More informationGC-xt. The most flexible GC /GC-MS liquid sample injector
GC-xt Prep and Load Platform The most flexible GC /GC-MS liquid sample injector Environmental Foods/Beverages Consumer Products Forensics Petrochemicals/Polymers Pharmaceuticals GC-xt Liquid mode Prep
More informationAN INTRODUCTION TO HEADSPACE SAMPLING IN GAS CHROMATOGRAPHY FUNDAMENTALS AND THEORY. Andrew Tipler
AN INTRODUCTION TO HEADSPACE SAMPLING IN GAS CHROMATOGRAPHY FUNDAMENTALS AND THEORY Andrew Tipler Chromatography Research and Technology Manager PerkinElmer, Inc. Table of Contents Introduction 3 Fundamental
More informationSplit / Splitless Injection for Capillary GC
Split / Splitless Injection for Capillary GC Speakers John V Hinshaw CHROMacademy GC Dean GC Connections editor Moderator Tony Taylor CHROMacademy Trainer Technical Director, Crawford Scientific Dave Walsh
More informationExtraction, Derivatization and Ultra-Sensitive GC/Triple Quadrupole Analysis of Estrone and Estradiol in Human Serum
Extraction, Derivatization and Ultra-Sensitive GC/Triple Quadrupole Analysis of Estrone and Estradiol in uman Serum Technical verview Clinical Research Authors Anthony Macherone, Ph.D. Agilent Technologies,
More informationAnalysis of Liquid Samples on the Agilent GC-MS
Analysis of Liquid Samples on the Agilent GC-MS I. Sample Preparation A. Solvent selection. 1. Boiling point. Low boiling solvents (i.e. b.p. < 30 o C) may be problematic. High boiling solvents (b.p. >
More informationAromatic plants: from extraction to analysis
Aromatic plants: from extraction to analysis Thierry TALOU Agro-industrial Chemistry Laboratory National Polytechnic Institute of Toulouse ENSIACET 4 allée Emile Monso 31432 Toulouse Olfactory system Olfactory
More informationRapid and Reproducible Amino Acid Analysis of Physiological Fluids for Clinical Research Using LC/MS/MS with the atraq Kit
Rapid and Reproducible Amino Acid Analysis of Physiological Fluids for Clinical Research Using LC/MS/MS with the atraq Kit Fast, simple and cost effective analysis Many areas of biochemical research and
More informationNANOCOMPOSIX'S GUIDE TO ICP-MS MEASUREMENT
NANOCOMPOSIX'S GUIDE TO ICP-MS MEASUREMENT AND ANALYSIS SEPTEMBER 2012, V 1.1 4878 RONSON CT STE K SAN DIEGO, CA 92111 858-565 - 4227 NANOCOMPOSIX.COM Note to the Reader: We at nanocomposix have published
More informationAutomation of Solid Phase Extraction and Column Chromatographic Cleanup
Automation of Solid Phase Extraction and Column Chromatographic Cleanup Haibin Wan Ltd. Problems with Manual Operation 1. Unstable flow rate affects reproducibility and throughput. 2. Not convenient for
More informationGENERAL UNKNOWN SCREENING FOR DRUGS IN BIOLOGICAL SAMPLES BY LC/MS Luc Humbert1, Michel Lhermitte 1, Frederic Grisel 2 1
GENERAL UNKNOWN SCREENING FOR DRUGS IN BIOLOGICAL SAMPLES BY LC/MS Luc Humbert, Michel Lhermitte, Frederic Grisel Laboratoire de Toxicologie & Génopathologie, CHRU Lille, France Waters Corporation, Guyancourt,
More informationGas Chromatography. Gas Chromatograph
Gas Chromatography Gas Chromatograph Chromatography: Separate analytes in a mixture with a resolution 1.5 in the shortest amount of time and detection of separated components. 1 = m.p. 6 2 4 5 3 Gas supplies
More informationThis study was performed by Patrick Sullivan and staff at TestAmerica Analytical Testing Corp., Westfield, MA, USA
An Automated Method for the Fractionation of Extractable Petroleum Hydrocarbons (EPH) from Water and Soil Extracts Using the Gilson GX-274 ASPEC System Keywords: Aliphatic Hydrocarbons, Aromatic Hydrocarbons,
More informationExtraction 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 informationAppNote 1/2012. Rapid Cleanup and Comprehensive Screening of Pain Management Drugs in Urine using Automated Disposable Pipette Extraction and LC-MS/MS
AppNote 1/2012 Rapid Cleanup and Comprehensive Screening of Pain Management Drugs in Urine using Automated Disposable Pipette Extraction and LC-MS/MS Oscar G. Cabrices, Fred D. Foster, John R. Stuff, Edward
More informationDRUG METABOLISM. Drug discovery & development solutions FOR DRUG METABOLISM
DRUG METABLISM Drug discovery & development solutions FR DRUG METABLISM Fast and efficient metabolite identification is critical in today s drug discovery pipeline. The goal is to achieve rapid structural
More informationMaking the Leap to LC/MS/MS: Enhancing and Accelerating Clinical Research and Forensic Toxicology Applications
Making the Leap to LC/MS/MS: Enhancing and Accelerating Clinical Research and Forensic Toxicology Applications Introduction The resolving power of chromatography combined with the sensitivity and selectivity
More informationThermo Scientific Prelude SPLC System FPO. Making LC/MS accessible. to clinical research and toxicology labs
Thermo Scientific Prelude SPLC System FPO Making LC/MS accessible to clinical research and toxicology labs Specifically designed to make the power of LC/MS accessible Analysis of target compounds in complex
More informationLecture Chromo-3: Gas Chromatography. CHEM 5181 Fall 2004 Mass Spectrometry & Chromatography. Jessica Gilman and Prof. Jose-Luis Jimenez CU-Boulder
Lecture Chromo-3: Gas Chromatography CHEM 5181 Fall 2004 Mass Spectrometry & Chromatography Jessica Gilman and Prof. Jose-Luis Jimenez CU-Boulder Outline Introduction Instrument overview Carrier gas Sample
More information