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32 Pharmaceutical Technology REGULATORY SOURCEBOOK SEPTEMBER 2021 P h a r mTe c h . c o m Best Practices: Part 1 method, starting from the original [homogeneous] sam- ple" (16). The nomenclature used within the FDA guide- line is not consistent, hence the author added the term 'homogeneous' for clarity. This latter paragraph wording is similar to that of the USP General Notices but uses the term 'reportable result' in place of 'reportable value'. In general, the nomenclature used is in- consistent and confusing especially the term 'Original sam- ple from the lot' which is the Laboratory Sample (Table VI). GOODSamples Guideline 2015 (Food and Feed) In October 2015, the Sampling and Sample Handling Work- ing Group of the Association of American Feed Control Officials (AAFCO) produced a guideline, GOODSamples: Guidance on Obtaining Defensible Samples (17). This 83- page guideline was developed by a consortium led by FDA with the objective to "improve analytical data equivalency among state, federal and local agencies ... Because analytical data is only as good as the quality of the sample" (17). FDA's Center for Food Safety and Applied Nutrition rec- ognized the necessity for sampling integrity and embraced the theory of sampling. Francis Pitard, author of Pierre Gy's Sampling Theory and Sampling Practice (3) was the techni- cal reviewer of the AAFCO guideline. Unfortunately, FDA has not provided an equivalent sampling guideline for drug substances and drug products. Figure 3 compares sampling nomenclatures for Phase 1 across the IUPAC, ASTM, WHO, and AAFCO documents. The AFFCO guideline is closest to the WHO guideline in its simplicity of a seven-stage approach to sampling, although there are distinct differences in the nomenclature employed. These AFFCO definitions are shown in Table VII. Apart from the anomalous nomenclature of Term 1, the others are well recognizable (Table VIII). For example, the sam- pling of a solid, in this instance grain, is illustrated together with a possible analogous example for tablet production. Table Vll. Terms abstracted from the Association of American Feed Control Officials' GOODSamples: Guidance on Obtaining Defensible Samples (17). ID Title of Term Term Definition 1 Decision unit 1_Decision Unit The material from which a sample is collected and to which an inference is made 2 Increments 2_Increments An individual portion of the material collected by a single operation of a sampling device and combined with other increments to form a sample 3 Primary sample 3_Primary sample The collection of one or more increments taken from a decision unit according to a sampling protocol 5 Laboratory sample 5_Laboratory sample Material received by the laboratory 6 Analytical sample 6_Analytical sample results from any manipulation of a laboratory sample 7 Test portion 7_Test Portion The quantity of the material taken for measurement Table VIII. Comparison of sampling terms used for feed and pharmaceutical tablets. Term AFFCO Example Tablet Production Example Decision unit Truckload of grain Production batch of tablets Increments Individual probes of grain Stratified samples of tablets collected Primary sample All increments combined Composite of stratified tablet samples Laboratory sample Packaged and received by the Laboratory Random subsample of primary sample Analytical sample Grain prepared for testing Grind 20 tablets randomly selected. Test portion Mass taken for the analytical test Portion of the tablet grind for the analysis Table VI. Terms abstracted from FDA's Guidance for Industry, Investigating Out-of-Specification (OOS) Test Results for Pharmaceutical Production (16). Term Definition Individual sample preparation A prepared and/or treated solution of an aliquot which is measured in accordance with the test method (procedure) Replicate measurements Number of measurements from each individual sample preparation Original sample from the lot The sample submitted to the laboratory in accordance with the sampling plan [Laboratory Sample] in accordance with 21 Code of Federal Regulations ยง211.160 Aliquot Portion of the original sample composite used for an individual sample preparation as specified in the test method Test method (procedure) Written and approved instructions for the performance of an analytical testing procedure including the number of individual sample preparations and replicate measurements together with acceptance criteria and the formula for calculating the reportable result