气相色谱-三重四极杆质谱法测定液体乳及乳粉中的17种邻苯二甲酸酯类增塑剂

Determination of 17 kinds of phthalic acid esters in milk and milk power by gas chromatography-tandem mass spectrometry

目的建立气相色谱-三重四极杆质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定液体乳及乳粉中17种邻苯二甲酸酯类增塑剂的含量。方法样品经乙腈超声提取,凝胶渗透色谱(gel permeation chromatography,GPC)净化后用GC-MS/MS分析,外标法定量。结果该方法线性关系良好,相关系数为0.9956～0.9999;方法的检出限(S/N=3)为3～60μg/kg;定量限(S/N=10)为10～200μg/kg;在50、200、500μg/kg添加水平下的平均回收率为78.2%～115.4%,相对标准偏差为2.65%～9.95%。结论本研究建立的方法样品处理简单快速、净化效果好、灵敏度和选择性高,适用于日常检测工作。

Objective To establish a method for simultaneous determination of 17 kinds of phthalic acid esters(PAEs) in milk and milk power by gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods Samples were extracted by acetonitrile and purified by gel permeation chromatography(GPC). Than they were analyzed by GC-MS/MS with external standard method. Results The linear relation of this method was good with the correlation coefficients of 0.9956-0.9999. The limits of detections(LODs, S/N=3) for 17 kinds of PAEs were in the range of 3-60 μg/kg, and the limits of quantitations(LOQs, S/N=10) were in the range of 10-200 μg/kg. The average recoveries of 17 kinds of PAEs at 3 spiked levels of 50, 200, 500 μg/kg were 78.2%-115.4%, with relative standard deviations of 2.65%-9.95%. Conclusion This method is simple, rapid, sensitive and reliable, which is suitable for the simultaneous identification and quantification of 17 kinds of PAEs in milk and milk power.