Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Jungong 300, Shanghai 200090, P. R. China.
School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418, P. R. China.
J Agric Food Chem. 2023 Oct 18;71(41):15388-15397. doi: 10.1021/acs.jafc.3c05230. Epub 2023 Oct 5.
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 -(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.
本研究开发了一种新颖的、简化的衍生化方法和快速的样品前处理过程，采用碳纤维作为吸附剂，通过高效液相色谱-串联质谱法（HPLC-MS/MS）测定酱油中的 3-氯-1,2-丙二醇（3-MCPD）。首先，3-MCPD 用碳纤维进行富集和纯化，然后用甲醇-水溶液洗脱。随后，用（二甲氨基）-苯酚对分析物进行衍生化，通过 HPLC-MS/MS 进行灵敏检测。3-MCPD 的检测限和定量限分别验证为 0.5 和 1.0μg/kg。加标实验显示回收率在 83%至 94%之间，相对标准偏差≤10%。该方法进一步用有证参考物质进行了验证。此外，还使用该方法测试了来自当地市场的 11 个实际酱油样品。这些结果揭示了 3-MCPD 的广泛污染。因此，本研究为酱油中 3-MCPD 的灵敏、准确和精确测定提供了一种较好的替代方法。
