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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。
Objective: To understand the effect of solid-phase extraction cartridge on the determination of 3-chloro-1,2-propanediol in condiment. Methods: The sample was pretreated by solid-phase extraction cartridge instead of traditional matrix solid-phase dispersion extraction. The sample was purified with n-hexane, eluted with ether, combined with triethylamine-catalyzed derivatization of heptafluorobutyric anhydride (HFBA-Et3N) -MS measurement. Results: The experimental results showed that the SPE cartridge has a good purification effect on the sample, which is basically consistent with the national standard method, and there is no significant difference (t> 0.05). The three spiked levels Rates ranged from 91.6% to 108.2% with relative standard deviations between 3.05% and 8.79% (n = 6). Conclusion: The method is simple, rapid, accurate and economical, suitable for the detection of 3-MCPD in condiments.