AOAC Gluten Quantitative Validation Guidance-Round 1(Nov 2023)

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LOD and LOQ will be estimated using reproducibility data (S R and RSD R ).

Data collected from analysis of incurred test materials for all matrices will be used to model the relationship between analyte 614 concentration and reproducibility. Data used must meet other method performance criteria (e.g., recovery). 615 616 and intermediate precision standard deviation must be taken into account in the estimation of LOD (also referred to as a precision 617 profile estimation method for LOD). Full instructions for the calculations to estimate LOD are in Annex D. 618 LOQ estimation will be based on the relationship between concentration and intermediate precision standard deviation. Full 619 instructions for the calculations to estimate LOQ are in Annex D. 620 6.6 Acceptance Criteria 621 All parameter point estimates must meet any applicable requirements for confidence intervals established by the AOAC 622 Statistics Committee or other relevant reviewers. 623 If an applicable SMPR is available for a method, the collaborative study data must meet the corresponding criteria. 624 In the absence of an applicable SMPR, an expert review panel will evaluate the study data according to their expert opinions. 625 LOQ 626 The LOQ must be greater than or equal to the LOD. 627 The RSD R at the LOQ must be less than or equal to the RSD R in the relevant SMPR. If there is no SMPR available, RSD R at the 628 LOQ must be ≤ 30%. 629 If a method developer has an LOQ claimed as part of the method design (e.g., the lowest non-zero calibrant), the estimated 630 LOQ from the Collaborative Study (which meets the SMPR requirements for maximum RSD R ) must be less than or equal to the 631 claimed LOQ of the kit, within statistical tolerances. If the estimated LOQ from the Collaborative Study is greater than the claimed 632 LOQ of the kit, the method developer must revise the LOQ claimed in the test kit insert and validation reports to meet the 633 precision requirements for LOQ. 634 In the validation reports and test kit inserts, the method developers must indicate the actual RSD R value estimated for the 635 LOQ of the kit as part of the LOQ information. For example: 636 LOQ 15 , for a method where the existing LOQ claimed by the kit had an estimated RSD R of 15% in the Collaborative Study 637 LOQ 30 , for a method where the LOQ was set based on the Collaborative Study outcome and a maximum RSD R of 30% 638 Acceptance criteria for the maximum RSD also includes meeting requirements for confidence intervals, as established by the 639 AOAC Statistics Committee. 640 6.7 Collaborator Comments 641 Comments on the candidate method should be encouraged from all collaborators, and any comments should be reported 642 in the collaborative study report. 643 LOD will be estimated using a hypothesis test approach, with α = β = 0.05. The relationship between observed concentration

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7. Matrix Extension

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7.1 Matrix Extension for single lab validation studies

A single lab matrix study must be performed as described in 4.4, picking up where the laboratory left off in the gluten source 646 tables (1 and 2). A matrix study must also be completed by an independent laboratory, and reported, as described under 5.2 . 647 7.2 Matrix Extension for multi-site collaborative studies 648 A single lab matrix study must be performed as described in 4.4, picking up where the laboratory left off in the gluten source 649 tables (1 and 2). A minimum of eight collaborator sites will perform the matrix studies as described under 6.3 and reported as 650 described under 6.5 .

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