婴幼儿配方乳粉中氯丙醇酯和缩水甘油酯的含量测定

Determination of chloropropyl ester and glycidyl ester in infant formula milk powder

目的:建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定婴幼儿配方乳粉中氯丙醇酯(chloropropanol ester,MCPDE)和缩水甘油酯(glycidyl ester,GE)的分析方法。方法:通过碱水解提取婴幼儿配方奶粉中脂肪,采用固相萃取净化,旋蒸浓缩,应用气相色谱-四极杆串联质谱法测定MCPDE和GE。结果:婴幼儿配方奶粉中3-MCPDE、2-MCPDE和GE的检出限分别为4、8、2μg/kg,在0~600μg/kg的线性范围内,线性相关系数大于0.999,在奶粉样品中添加20、100、200μg/kg 3个浓度水平的平均加标回收率在82.1%~106.9%,相对标准偏差不大于9.0%。运用该方法测定32份婴幼儿配方乳粉中MCPDE和GE的测定,结果表明90.0%以上的婴幼儿配方乳粉检出该类污染物质。结论:该方法准确度高,重现性好,能够满足配方乳粉中MCPDE和GE的检测要求。

Objective:To establish a method for determination of chloropropanol ester(MCPDE)and glycidyl ester(GE)in infant formular by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods:The fat in infant formula was extracted by alkali hydrolysis,purified by solid phase extraction,and concentrated by rotary steam.MCPDE and GE were determined by gas chromatography-quadrupole tandem mass spectrometry.Results:The limits of detection of 3-MCPDE,2-MCPDE and GE in infant formula were 4,8 and 2μg/kg.The linear correlation coefficient was greater than 0.999 in the linear range of 0-600μg/kg,the average recoveries from the infant formula at the 3 concentraton levels of 20,100,200μg/kg were in the range of 82.1%-106.9%,and the relative standard deviations were no more than 9.0%.This method was applied to the determination of MCPDE and GE in 32 infant formula,and the results showed that more than 90.0%of infant formula was detected with these pollutants.Conclusion:The method has accurate and reproducible,which can meet the requirements of MCPDE and GE in infant formula.