AOAC_guidlines_for_single_laboratory_validation_of_chemical_methods_for_dietary_supplements.pdf

AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals CONTENTS 1.0 Introduction 1.1 Definitions 1.1.1 Validation 1.1.2 Method of analysis 1.1.3 Performance characteristics of a method of analysis 2.0 Single-Laboratory Validation Work 2.1 Preparation of the Laboratory Sample 2.2 Identification 2.3 Method of Analysis or Protocol 2.3.1 Optimization 2.3.2 Reference standard 2.3.3 Ruggedness Trial 2.3.4 Specific variables a. Analyte addition b. Reextraction of the extracted residue c. Comparison with different solvents d. Comparison with results from a different procedure e. System Suitability Checks 3.0 Performance Characteristics 3.1 Applicability 3.2 Selectivity 3.3 Calibration 3.3.1 External Standard Method 3.3.2 Internal Standard Method 3.3.3 Standard Addition Method 3.4 Reliability Characteristics 3.4.1 Accuracy 3.4.2 Repeatability Precision sr, RSDr 3.4.3 Measurement Uncertainty 3.4.4 Reproducibility Precision sR, RSDR 3.4.5 Intermediate Precision 3.4.6 Limit of Determination 3.4.7 Reporting Low-level Values 3.4.8 Dichotomous Reporting 3.5 Controls 3.5.1 Control Charts 3.5.2 Injection Controls 3.5.3 Duplicate Controls 3.6 Confirmation of Analyte 1 2002-12-19 4.0 Report as applicable Identity, source, purity of reference material Scope, applicability, nonapplicability Recovery, levels, percent n 5 at each concentration level Repeatability, RSDr n 5 at each concentration level Intermediate precision, RSDi n 5 at each concentration level Limit of determination Because of the time and expense required for the determination of modern analytes such as pesticide residues, industrial contaminants, veterinary drugs, allergens, botanicals, dietary supplements, and alternative medicines in complex matrices, there is considerable interest in obtaining acceptable methods of analysis faster and cheaper. It has been suggested that accreditation of labor