SPE小柱在调味品3-氯-1,2-丙二醇检测中的应用研究

目的:了解固相萃取小柱在调味品3-氯-1,2-丙二醇测定中的应用效果。方法:采用固相萃取小柱替代传统的基质固相分散萃取技术对样品进行前处理,用正己烷净化,乙醚洗脱,结合三乙胺催化的七氟丁酸酐(HFBA-Et3N)衍生,GC-MS测定。结果:实验结果表明,SPE小柱对样品的净化效果较好,与国标法比较测定结果基本一致,t检验无显著性差异(P>0.05),对5种调味品的三个加标水平回收率在91.6%～108.2%之间,相对标准偏差在3.05%～8.79%之间(n=6)。结论:该方法简单、快速、准确、经济,适用于调味品中3-MCPD的检测。

The application of solid phase extraction column in determination of 3-monochloropropane-1,2-diolt in condiments

Objective:To evaluate the value of solid phase extraction column for determination of 3-monochloropropane-1,2-diolt in condiments.Methods:Samples were transferred to SPE column after addition of internal standard d5-3-MCPD,from which samples were purified with n-hexane and then extracted with ethyl ether.Heptafluoroheptabutyric acid anhydride amended with triethylamine(HFBA-Et3N) was added to the sample to derive chloropropanols,then the derivative analytes were analyzed by GC-MS.Results:The determined results by this method were in consistent with those by the international method(P>0.05),the recovery was 91.6%~108.2%,the RSD was 3.05%~8.79%(n=6),and better purification effect was obtained.Conclusion:The method is reliable,fast and economical for routine determination of 3-MCPD in condiments.