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Rapid Sample Enrichment, Novel Derivatization, and High Sensitivity for Determination of 3-Chloropropane-1,2-diol in Soy Sauce via High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Yunyu Tang, Guangxin Yang, Xiaoxia Liu, Lixia Qin, Wenlei Zhai, Essy Kouadio Fodjo, Xiaosheng Shen, Yuan Wang, Xiaoyi Lou, Cong Kong

2023Journal of Agricultural and Food Chemistry39 citationsDOI

Abstract

A novel, simplified derivatization method and a rapid sample preparation process using carbon yarn as a sorbent for the determination of 3-chloropropane-1,2-diol (3-MCPD) in soy sauce via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) was developed. 3-MCPD was first enriched and purified with carbon yarn and then eluted with a methanol–water solution. Subsequently, the analyte underwent derivatization with p -(dimethylamino)-phenol for sensitive detection via HPLC-MS/MS. The limit of detection and the limit of quantitation for 3-MCPD were validated to be 0.5 and 1.0 μg/kg, respectively. Spiking experiments showed recoveries between 83 and 94%, with a relative standard deviation of ≤10%. The method was further validated with a certified reference material. Furthermore, 11 real soy sauce samples from local markets were tested by using this method. These results reveal the widespread 3-MCPD contamination. Consequently, this study offers a preferable alternative for the sensitive, accurate, and precise determination of 3-MCPD in soy sauce.

Topics & Concepts

ChromatographyDerivatizationDetection limitChemistryAnalyteHigh-performance liquid chromatographyMass spectrometryTandem mass spectrometryElutionLiquid chromatography–mass spectrometrySample preparationDye analysis and toxicityPesticide Residue Analysis and SafetyAnalytical chemistry methods development