三重四极杆气质联用法测定白酒中的16种邻苯二甲酸酯类增塑剂
Simultaneous determination of 16 kinds of phathalate plasticizers in wine by gas chromatography /triple quadrupole mass spectrometry
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摘要: 建立了一种可用于白酒中邻苯二甲酸酯类增塑剂检测的三重四极杆气质联用(GC-MS/MS)分析方法。白酒除去乙醇后,采用正己烷提取,采用GC-MS/MS的多反应监测模式,以保留时间和离子对(母离子和子离子)信息来定性,以母离子和响应值高的子离子进行定量。结果表明,该方法的检测限为0.4ng/g,相对标准偏差为1.74%4.95%,目标化合物的回收率为84%118%;该方法快速准确可用于白酒中的增塑剂的定性确认和含量测定。Abstract: A rapid and accurate method was established based on chromatography /triple quadrupole mass spectrometry ( GC-QqQ-MS/MS) to simultaneously determine 16 kinds of phthalate plasticizers in wines.To- bemeasured wine samples were extracted with hexane and separated with an TG- 5MS analytical column ( 30m ×0.25mm ( internal diameter) × 0.25μm film thickness) . The QqQ mass spectrometer was operated in a multiplereaction monitoring mode.The qualitative analysis of the samples was carried out by comparing the retention-time and ion-pair with that of standard material, and the quantitative analysis was carried out by the abundance of the ion-pair with that of the standard material.Results indicated that the limits of detection for phathalates in the test samples were 0.4ng /g; the relative standard deviation was in the range of 1.74% 4.95%, and the recoveries were in the range of 84% ~ 118%. The present method could be applied for the routine analysis of the 16 kinds of phthalate plasticizers in wines.