MCPD-02 Reviewer Forms (July 19, 2018)

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Reviewer 4 Expert Review Panel for Infant Formula and Adult Nutrition (MCPD)

Evaluation of Method __ MCPD-02

Title: 2-Monochloropropanediol (2-MCPD), 3-Monochloropropanediol (3-MCPD) and Glycidol in infant formula and adult/pediatric nutritional formula

Author: Jan Kuhlmann

Reviewer Name:

Summary of Method: Free and bound analytes are extracted from powder samples liquid samples. For powder infant formula, free and ester-bound analytes are extracted by triple Heat-Ultrasonic-Pressure- supported Solvent Extraction using methanol and tert-butyl-Methyl-Ether (t-BME). By application of a subsequent liquid-liquid extraction with saturated soldium sulfate and isohexane/t-BME, the combined extracts are separated into a polar fraction containing the 2- and 3-MCPD and a non-polar fraction containing the ester-bound analytes. For liquid samples, a flocculation followed by washing step is used as a pre-treatment, before involving a liquid-liquid extraction with Diethyl ether to extract free form. Extraction of ester bound analytes is performed in liquid samples by Rose-Gottlieb approach. Free 2-MCPD and 3-MCPD from liquid or powder samples are derivatized using phenylboronic acid (PBA) and measured against their derivatives by GC/MS. Ester bound forms of 2-MCPD, 3-MCPD and GE are analyzed after release of the free form by an overnight alkaline transesterification. Hydrolysis is stopped by use of an acidic solution containing NaBr for stabilization of glycidol through conversion to Monobromopropanediol. Analytes are then derivatized using PBA and measured against their derivatives by GC/MS.

Method Scope/Applicability: Powder and liquid infant formula and adult/pediatric nutritional formula.

General comments about the method: Method

Method Clarity:

1