Analytical Method Validation

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1 Analytical Method Validation A. Es-haghi Ph.D. Dept. of Physico chemistry vaccine and serum research institute

2 Introduction Test procedures for assessment of the quality levels of pharmaceutical products are subject to various requirements The CGMP regulations [21 CFR (a)] require that test methods, which are used for assessing compliance of pharmaceutical products with established specifications, must meet proper standards of accuracy and reliability according to these regulations [21 CFR (a)(2)], users of analytical methods described in the USP and the NF are not required to validate accuracy and reliability of these methods, but merely verify their suitability under actual conditions of use Recognizing the legal status of USP and NF standards, it is essential, therefore, that proposals for adoption of new or revised compendial analytical methods be supported by sufficient laboratory data to document their validity ٢

3 What is Validation? USP 30-NF 25, General Chapter <1225> Validation of Compendial Methods Validation of an analytical method is the process by which it is established, by laboratory studies, that the performance characteristics of the method meet the requirements for the intended analytical applications. ICH Guideline Q2A Text on Validation of Analytical Procedures The objective of validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose. FDA draft guidance Analytical Procedures and Method Validation Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use. ٣

4 Analytical Method Validation In actual practice, analytical methods validation involves Established analytical method Data from controlled samples Statistical evaluation Assessment of performance characteristics and applicability ٤

5 USP Performance Characteristics Performance Characteristics are discrete attributes, derived by actual execution of an analytical method using controlled samples, which demonstrate the suitability and proper use of that method for a specific application ٥

6 USP Performance Characteristics SPECIFICITY LINEARITY RANGE DETECTION LIMIT QUANTITATION LIMIT ACCURACY PRECISION RUGEDNESS ROBUSTNESS SYSYEM SUITABILITY ٦

7 Specificity / Selectivity ICH Q2A and USP the ability to assess unequivocally the analyte in the presence of components that may be expected to be present, such as impurities, degradation products, and matrix components Lack of specificity of an individual analytical procedure may be compensated by other supporting analytical procedure(s) Other international authorities (IUPAC, AOAC) have preferred the term Selectivity reserving Specificity for those procedures that are completely selective ٧

8 Specificity Identification to ensure the identity of the analyte Purity Test accurate statement of the content of impurities of an analyte (related substances, heavy metals, residual solvents, etc.) Assay an exact result which allows an accurate statement on the content of potency of the analyte in a sample ٨

9 Specificity Some analytical procedures are not sufficiently specific for the intended purpose Assay by titration Assay of enantiomer by achiral method Identification by UV absorbance A combination of two or more analytical procedures is recommended to achieve sufficient specificity ٩

10 Specificity Should be one of the first validation items When the criteria are not met, this indicates that the method is not sufficiently developed Poor specificity can impact accuracy, precision and linearity ١٠

11 Linearity The ability to generate responses which are directly proportional to the concentration of an analyte in a sample ١١

12 Linearity A linear relationship requires fewer standards to define the response curve than a non-linear one justifies the use of a single point standard to quantitate across the range ١٢

13 Linearity USP <1225> Evaluated across the RANGE Visual examination of a plot of signals as a function of concentration Statistical evaluation of correlation coefficient, y-intercept, slope, and residual sum of squares of regression line or after mathematical transformation ICH Guidance Performed directly on the drug substance (dilution of standard stock solution) Separate weighing of synthetic mixtures of the drug components Minimum of five concentration is recommended ١٣

14 Linearity Required for Assays (Category I) Impurity tests (Quantitative Category II) May be for Performance Tests (Category III-Dissolution, etc.) Not required for Limit tests (Category II- Impurity Test) Identification ١٤

15 Range UPS <1225> The interval between the upper and lower quantitation levels of analyte (including these levels) demonstrated by suitable precision, accuracy, and linearity ICH Guidance The following minimum specified ranges should be considered Assay of drug substance or finished drug product from 80% to 120% of the test concentration Content Uniformity minimum of 70% to 130% of the test concentration, unless otherwise justified ١٥

16 Detection Limit/ Quantitation Limit Characteristic for low level impurity assays DL (LOD) the lowest amount of any analyte which can be detected but not necessarily quantitated QL (LOQ) the lowest amount of analyte that can be determined with acceptable precision and accuracy ١٦

17 Determination of Detection Limit Non-instrumental Methods analysis of samples with known concentrations of analyte to establish the minimum concentration at which the analyte can be reliably (the ability to reproducibly obtain a signal for the analyte) detected Examples TLC, titrations, color compositions Instrumental Same as for non-instrumental methods, plus estimation of the DL can be made at a value at which the signal to noise ratio (S/N) is 2:1 or 3:1 ١٧

18 Estimation of DL (ICH) DL = 3.3 σ/s Where: σ = Standard deviation ( noise ) of response S = slope of the calibration curve for linearity DL can be based on any of the following σ of the blank σ of the lowest level linearity point the calibration plot (regression) ١٨

19 Quantitation Limit Definition USP <1225> the lowest amount of analyte in a sample that can be determined with acceptable precision and accuracy under the stated experimental conditions Essentially identical to ICH Q2A Quantitation Limit (QL) = Limit of Quantitation (LOQ) ١٩

20 Determination of QL Non-Instrumental from analysis of samples with appropriate minimum level of analyte quantified with acceptable accuracy and precision Instrumental same as non-instrumental, plus estimation of the QL can be made at a value at which the signals to noise is 10:1 ٢٠

21 Estimation of QL (ICH) QL = 10 σ/s where σ = standard deviation of response S = slope of the calibration curve for linearity σ can be based standard deviation of the blank or of the lowest level linearity point ٢١

22 Case Study ٢٢

23 Accuracy Definition USP The closeness of the result obtained by the method to the true value. ICH The closeness of the result obtained by the method to a value that is accepted as conventionally true value or as a reference value. ٢٣

24 Accuracy The accuracy of an analytical method should be established across its range ICH recommends a minimum of 9 determinations over a minimum of 3 concentrations covering the stated quantitation range (3 test at 3 conc.) Accuracy is calculated as the percentage of recovery by the assay of the known added amount of analyte in the sample the difference between the mean and the accepted true value, together with confidence intervals ٢٤

25 Accuracy 5 ways to determine the Accuracy Testing of a Reference Standard Mixture with Excipients (Spiked placebo) Standard addition (Spiked sample) Inferred from linearity and specificity data Comparison with a method known to be accurate (reference method) ٢٥

26 Accuracy assay of a drug substance Testing of a Reference Standard Comparison with a reference standard method ٢٦

27 Recovery of Drug F Ref Std at different levels ٢٧

28 Comparison with Reference Method There is no difference with p < 0.05 ٢٨

29 Precision The degree of agreement among results from individual samplings of a homogeneous sample ٢٩

30 Precision Precision is expressed as RSD Precision should be evaluated across the specified Quantitation range of the method Determination Assay individual samples of a homogeneous preparation Calculate Standard Deviation or Relative Standard Deviation Method precision should include all sources of variation from sample preparation to rounding the final test result ٣٠

31 Precision ICH recommends a minimum of 9 determinations over a minimum of 3 concentrations covering the stated quantitation range (3 test at 3 conc.) OR Using a minimum of 6 determinations at 100% of the test concentration ٣١

32 ICH-USP Level of Precision Repeatability agreement within a short period or the same analyst and instrumentation Intermediate precision agreement in results intra-laboratory but from different days, analysts and equipment (as appropriate) Reproducibility agreement in results between laboratories (as in a collaboration study) ٣٢

33 Precision vs. Ruggedness In USP, Reproducibility and intermediate precision are also considered together with Ruggedness ٣٣

34 Precision choice of acceptance criteria Practical Considerations Ability to meet criteria may be instrument dependent Maximum acceptance criteria for precision should be linked to acceptance criteria for claim or specification to be able to obtain a reliable result (reduce Out-Of Specifications) ٣٤

35 Precision Repeatability (5 replicate injections) Assay Limit (%) Max, % RSD Impurities (depending on level) 5 to 25 ٣٥

36 Precision choice of acceptance criteria Intermediate Precision FDA recommends a minimum of 2 different days with different analysts Acceptance criteria Perform F-test results between labs should not be statistically different Typically about 2x repeatability (2 x RSD) However, a statistical difference may still not be significant (practical consideration). Need to evaluate suitability for methods intended use ٣٦

37 Reproducibility Precision FDA at least 2 laboratories within the company FDA for multi-laboratory follow ASTM 691 Standard practice for conducting an laboratory study to determine the precision of a test method AOAC Protocol 8 samples, 8 laboratories ٣٧

38 Ruggedness Reproducibility with the same samples using different laboratories, analysts, days, reagent lots (same brand), and environmental conditions Precision should be evaluated across the specified Quantitation range of the method ٣٨

39 Ruggedness vs. Robustness Reproducibility of the test results under conditions normally expected from laboratory to laboratory and from analyst to analyst Method parameters are kept constant (difference with robustness) ٣٩

40 Ruggedness Determination Analysis of an homogeneous sample in different laboratories, by different analysts, under prevalent environmental conditions using the specified parameters The degree of reproducibility of test results is determined as function of the variables ٤٠

41 Ruggedness study normal variables Analyst A, B, C Day 1, 2, 3 Lab L, M N Column X, Y, Z Selected comparisons are evaluated since evaluating all possible variations would require 81 experiments (3 x 3 x 3 x 3) The influence of each variable may be evaluated using a multifactor experimental design (Plackett- Burman, Hendrix, etc.) ٤١

42 Ruggedness Degree of reproducibility of test results as a function of the variables ٤٢

43 Robustness The ability to remain unaffected by small but deliberate variations in method parameters- evaluates reliability Provides an indication of the reliability of the method during normal usage ٤٣

44 Robustness Evaluated by varying method parameters and determining the effect (if any) on the results of the method It should be considered early in the development of a method If the results are susceptible to parameter variations, these parameters should be adequately controlled and a precautionary statement included in the method ٤٤

45 Robustness Two approaches Uni-variable Systematically varying each parameter sequentially Typically, each parameter may be varied by 5 10% above and below the value set in the method Multi-variable Use of the statistical design Central Composites Fractional factorials, Two-factor Plackett-Burman statistical approach Hendrix ٤٥

46 System Suitability Ensures that both methodology and instrumentation are performing within expectation prior to the analysis of the test samples USP General Chapter <1225> System suitability tests are based on the concept that the equipment, electronics, analytical operations, and samples to be analyzed constitute an integral system that can be evaluated as such. System suitability test parameters to be established for a particular procedure depend on the type of procedure being evaluated. They are especially important in the case of chromatographic procedures. ٤٦

47 System Suitability Provides assurances that the system is working at the time of analysis Ensures that both methodology and instrumentation are performing within expectations prior to the analysis of the test samples Should be monitored during run time to verify that criteria remain realistic and achievable ٤٧

48 System Suitability Parameters for chromatographic method Resolution specificity Column efficiency specificity Relative standard deviation precision Tailing factor accuracy and precision QL sensitivity Capacity factor specificity Reference Standard Check - analyte ٤٨

49 USP Method Categories Category I Quantitative test for major active ingredients (chromatographic and titration) Category II Impurities or degradation compounds; quantitative or limit tests Category III performance tests (dissolution, drug release, tapped density, particle size) Category IV Identification tests (TLC, IR, UV, Chemical ID <191> ٤٩

50 USP <1225> Data Elements for Validation ٥٠

51 ICH Q2B Data Elements for Validation May be required, depending on the nature of the specific test Is not needed if reproducibility has been performed ٥١

52 Choice of Performance Characteristics Not all Performance Characteristics are needed to validate an analytical method or validated in the same way Determine the expected use of the test procedure (e.g., assay, dissolution, limit test, ID test) Take into account the type of analytical technique used (chromatographic, spectrophotometric, titration, etc.) Establish the requirements of the analytical application Degree of precision and accuracy needed The concentration range of the analyte The level of tolerable interference, if any ٥٢

53 Protocol for Final Validation Studies Initial analytical methods are often developed in R&D areas with some preliminary validation data These procedures can be slightly modified when transferred to QC areas for complete validation including multi-site collaborative studies ٥٣

54 Validation Protocols The validation protocol document contains Description of the analytical method and its intended use (purpose) List of applicable performance characteristics Appropriate acceptance criteria Review and approval signatures ٥٤

55 Pre-validation Assessment Equipment Suitable for expected accuracy? Reference Materials Suitability characterized? Analytical Method Is procedure finalized? Validation Protocol Management / QA approved? ٥٥

56 Pre-validation Assessment Equipment Demonstrate that equipment used in validation studies is suitable for use and is comparable to equipment used for routine analysis Calibrated (as applicable) Qualification should have been performed Installation Qualification Operation Qualification Performance Qualification Routine maintenance performed- proper working order ٥٦

57 Pre-validation Assessment Reference Materials evaluate suitability of use FDA requires no additional evaluation of USP Reference Standards Standardization of reagents vs. Primary standards when available (i.e., use of reagent grade chemical need qualification) Principal analyte (purity and homogeneity) Impurity Standards chemical purity is very critical if used to determine relative response Solution stability of standard preparations ٥٧

58 Pre-validation Assessment Analytical Method must be final before validation Individual procedure steps may impact overall method accuracy or precision Solution preparations concentration of analyte in solution for analysis (suitable range) System suitability necessary parameters and acceptance criteria must be specified Changes may negatively impact validation studies previously performed Later changes in tailing factor or resolution criteria from robustness evaluation may have a significant impact on integration in accuracy evaluations ٥٨

59 Standard and Sample Solution Preparation Overall method precision and accuracy are also impacted by sampling, weighing, and quantitative dilutions No instrumental technology can overcome these errors The precision and accuracy of a final analytical method can be better than the precision and accuracy of the preparation of the test solutions ٥٩

60 Revalidation Revalidation may be necessary in the following cases a submission to the USP of a revised analytical method use of an established general method with a new product or raw material The ICH documents give guidance on the necessity for revalidation in the following circumstances changes in the synthesis of the drug substance changes in the composition of the drug product changes in the analytical procedure ٦٠

61 RVSRI deffects in Analytical Method Validation Equipment Personnel Reference Materials Analytical Methods Validation Protocol Change control Weak links between different chain to final product be completely assured ٦١

62 Quick Quiz Cumulative errors in serial dilution To prepare 100 fold dilution of a stock solution, what is the most precise procedure when considering the necessary individual Class A pipette and volumetric flask tolerances? A. 1.0 ml/10 ml; 1.0 ml/10 ml B. 5.0 ml/50 ml; 5.0 ml/50 ml C ml/100 ml; 10.0 ml/100 ml D. 1.0 ml/100 ml E. 2.0 ml/200 ml F. 5.0 ml/500 ml ٦٢

63 Tolerance of Class A Glassware (see USP <31> Volumetric apparatus) ٦٣

64 Quick Quiz Cumulative errors in serial dilution Sum of step errors A. 1.0/10; 1.0/10L B. 5.0/50; 5.0/50 C. 10.0/100; 10.0/100 D. 1.0/100 E. 2.0/200 F. 5.0/ = ± 1.6% = ± 0.6% = ± 0.43% = ± 0.68% = ± 0.35% = ± 0.23% ٦٤

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