AOAC SPIFAN Nutrients ERP Reviewer Forms (December 7, 2022)

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Pros/Strengths: -The described method makes use of a selective detection method by MS together with the separation properties of a HILIC UHPLC column. -The robustness was tested against three different MS systems, two different LC columns, two different laboratories and three different analysts.

Supporting Data • General Comment:

Method Optimization: A calibration line is established on every analysis. The calibration line is analyzed before the analysis of samples and is based on seven concentrations from 0.03mg/L to 10.0 mg/L.

• Performance Characteristics:

Analytical Range: SMPR: 0.5-2500 mg/100 g Method: 0.5-110 mg/100 g

LOQ: SMPR: ≤0 .5 mg/100 g Method: 0.29 mg/100g

A method blank was spiked with a low concentration of taurine near the expected LOQ. Next to the spiked method blank a method blank was included to calculate the mean blank. A total of 24 measurements of spiked method blanks were performed over six days. The standard deviation of these analyses was calculated. The standard deviation was multiplied by three for the LOD (SLOD) and multiplied by ten for the LOQ (SLOQ). The LOD and LOQ were then determined by adding the SLOD and SLOQ to the blank mean.

Accuracy/Recovery : SMPR: 0.5-5.0 mg/100g 88-112% 5.0-150 mg/100g 90-110% 150-2500 mg/100g 93-107% Method: 92-105%

Reference materials NIST SRM 1869 and 1849a were used to assess the accuracy of the method based on their reference values of taurine. Both reference materials were analyzed on three days in triplicate. The determined accuracy of the method with NIST SRM 1849a is in good agreement with the reference value. The accuracy of the method with NIST SRM 1869 is lower than expected.

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