气相色谱 - 质谱仪测定植物油中氯丙醇酯  

Determination of MCPD Esters in Vegetable Oil by GC-MS

作　　者：栾田[1] 王晓婧[1] 廖雪 王缘[1] 赵岚[1] LUAN Tian;WANG Xiaojing;LIAO Xue;WANG Yuan;ZHAO Lan(Heilongjiang Provincial Center for Disease Control and Prevention,Harbin 150030,China)

机构地区：[1]黑龙江省疾病预防控制中心,黑龙江哈尔滨150030

出　　处：《现代食品》2022年第10期212-214,共3页Modern Food

摘　　要：目的:建立植物油中3-氯丙醇酯和2-氯丙二醇酯气相色谱-质谱检测方法。方法:植物油经溴代反应后,采用硫酸-甲醇溶液水解,经硅藻土固相萃取小柱净化,七氟丁酰基咪唑衍生后,采用气相色谱-质谱仪测定,以氘代同位素作为内标进行定量。结果:3-氯丙醇酯和2-氯丙二醇酯在10~300μg·kg^(-1)有良好的线性关系,相关性系数均大于0.999;3-氯丙醇酯和2-氯丙二醇酯的平均回收率分别为92.7%~102.7%和89.7%~108.2%,相对标准偏差分别为6.1%~9.8%和5.8%~9.3%,检出限均为0.020 mg·kg^(-1)。33份植物油样品中,3-氯丙醇酯检出率为93.94%,2-氯丙二醇酯检出率为72.73%。结论:建立的检测方法灵敏度高,准确可靠,适用于植物油中氯丙醇酯的检测,且植物油中氯丙醇酯检出率较高,存在一定的食品安全风险。Objective:To develop a method for determination of 3-MCPD esters and 2-MCPD esters in vegetable oil by gas chromatography-mass spectrometry.Method:After bromination,the vegetable oil was hydrolyzed by sulfuric acid-methanol solution,purified by diatomite solid phase extraction column,derivatized by HFBI,and determined by gas chromatograph-mass spectrometer with deuterated isotope as internal standard.Result:There was a good linear relationship between 3-chloropropanol ester and 2-chloropropanediol ester in the range of 10~300μg·kg^(-1),and the correlation coefficients were all greater than 0.999.The average recoveries of 3-chloropropanol ester and 2-chloropropanediol ester were 92.7%~102.7%and 89.7%~108.2%,respectively,and the relative standard deviations were 6.1%~9.8%and 5.8%~9.3%,respectively.The detection limits both were 0.020 mg·kg^(-1).The detection rates of 3-MCPDE and 2-MCPDE were 93.94%and 72.73%,respectively.Conclusion:The method is sensitive,accurate and reliable,and can be used for the determination of MCPD Esters in vegetable oils and fatty foods.

关 键 词：气质联用(GC-MS) 3-氯丙醇酯 2-氯丙二醇酯 植物油 内标法 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]