SPDS Lutein and Turmeric ERPs

Appendix K: Guidelines for Dietary Supplements and Botanicals

This appendix contains three complementary documents for the validation of dietary supplements and botanical methods: Part I: AOAC Guidelines for Single-Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals Part II: AOAC Guidelines for Validation of Botanical Identification Methods Part III: Probability of Identification: A Statistical Model for the Validation of Qualitative Botanical Identification Methods PART I AOAC Guidelines for Single-Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals 1.1 Definitions 1.1.1 Validation 1.1.2 Method of Analysis 1.1.3 Performance Characteristics of a Method of Analysis 2 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 Contents 1 Introduction

e. System Suitability Checks

3 Performance Characteristics 3.1 Applicability (Scope)

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 (s r 3.4.3 Measurement Uncertainty 3.4.4 Reproducibility Precision (s R 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

, RSD r

)

, RSD

)

R

3.5.2 Injection Controls 3.5.3 Duplicate Controls 3.6 Confirmation of Analyte 3.7 Stability of the Analyte

2.3.3 Ruggedness Trial 2.3.4 Specific Variables a. Analyte Addition

4 Report (as applicable) 4.1 Title 4.2 Applicability (Scope)

b. Reextraction of the Extracted Residue c. Comparison with Different Solvents d. Comparison with Results from a Different Procedure

4.3 Principle 4.4 Reagents 4.5 Apparatus 4.6 Calibration 4.7 Procedure 4.8 Calculations 4.9 Controls

Under a 5-year contract (2003–2008) with the National Institutes of Health-Office of Dietary Supplements, through the U.S. Food and Drug Administration, AOAC undertook an effort to validate methods for dietary supplement ingredients of interest. As part of the initiative, AOAC adapted and revised the traditional Official Methods SM process to include single-laboratory validation (SLV). Methods were first validated within a single laboratory to test their suitability and ruggedness without the complications of a multilaboratory collaborative study. SLVs proved to be an excellent debugging tool for complex methods; problems found within one laboratory could be dealt with so that a stronger method went on to the collaborative study. The SLV process, thus, became a step in preparation for the collaborative study. The SLV guidelines were approved by the AOAC Official Methods Board and Board of Directors in December 2002.

4.10 Results of Validation 4.10.1 Identification Data 4.10.2 Performance Data

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