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目的建立气相色谱-质谱测定植物油中氯丙醇酯的方法,并据此方法测定北京市售植物油中氯丙醇酯含量。方法样品用碱液水解后,经基质分散固相萃取净化,以七氟丁酰基咪唑(HFBI)衍生化后引入气相色谱-质谱仪,以内标校正,标准曲线法定量。结果 2-氯-1,3-丙二醇酯(2-MCPD)及3-氯-1,2-丙二醇酯(3-MCPD)在线性范围内的标准曲线线性相关系数>0.999;样品加标回收率在94%-122%之间,相对标准偏差<10%(n=6);使用FAPAS质控样品T2642QC进行测定,结果在允许范围之内。结论该方法简便、快速、准确,可满足植物油中氯丙醇酯检测的要求。
Objective To establish a method for the determination of chloropropanol esters in vegetable oils by gas chromatography-mass spectrometry and to determine the content of chloropropanol esters in vegetable oils sold in Beijing. Methods After the sample was hydrolyzed by lye, it was purified by matrix dispersive solid-phase extraction and derivatized with heptafluorobutanoyl imidazole (HFBI). The sample was then introduced into GC-MS and quantified by internal standard calibration and standard curve method. Results The calibration curves of 2-chloro-1,3-propanediol (2-MCPD) and 3-chloro-1,2-propanediol (3-MCPD) were linear within the linear range of> 0.999. Between 94% and 122%, the relative standard deviation was less than 10% (n = 6). The FAPAS control sample T2642QC was used to determine the result. The results were within the allowable range. Conclusion The method is simple, rapid and accurate and can meet the requirements of chloropropanol ester detection in vegetable oils.