AOAC SPSFAM PAC ERP

2. Is there information demonstrating that the method meets the SMPR Method Performance Requirements using the Reference Materials stated in the SMPR? If not, then specify what is missing and how this impacts demonstration of performance of the method. method performs within the SMPR Method Performance REquirements table specifications for all analytes in the SMPR applicability statement? If not, please specify what is missing and whether or not the method's applicability should be modified. 3. Is there information demonstrating that the

No reference materials were specified in the SMPR.

Below is how the method deviated from the SMPR:

1. LOQ: The LOQ's determined in this method are close to within range [0.05 mg/mL for juice (0.005%), 0.125 mg/g in dried products (0.0125%)] with dried products being slightly above the desired 0.01% 2. Analytical range: The method specifies 0.05 -10 mg/mL for procyanidin A2 and 0.01 -10 mg/mL for procyaindin B2, but do not specify for total procyanidins. If calculated for solid products this range would correspond to 0.0125% to 25% for procyanidin A2 and 0.025 to 25% for procyanidin B2. The is not up to the 55% specified in the SMPR. 3. Recovery: Recovery was outside the SMPR for dried and liquid spiked samples liquids 84 - 120 %, dried samples: 76.6 - 93.7% These values are much lower than specified by SMPR for individual procyanidins and no data was provided on total procyanidins. 4. RSDr: Precision was described for spiked samples as opposed to true samples. RSDs ranged from 6.1 to 13% for intra-day precision in dried samples and 3.6 to 16.5 % for liquid samples. All of the tests were performed on samples below 15% so no data collected for greater than 5%. The precision is close, but not within SMPR requirements of 10% for liquids and 15% for dried products. It would have been nice to see RSDs for the authentic samples. As well as RSDs for total procyanidins.

IV. General Submission Package

IV. General Submission Package 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional precautionary statements in the method? 2. Does the method contain system suitability tests or controls as specified by the SMPR? If not, please indicate if there is a need for such tests or controls and which ones.

No precautionary statements have been made. Statements should be added appropriately, especially regarding the use of concentrated acids and whether fume hoods are necessary for the thiolysis reaction.

No. Information regarding system suitability should be evaluated and added,