固相分散萃取-气相色谱-质谱法测定药酒中15种邻苯二甲酸酯的含量

Determination of 15 phthalate acid ester in medicinal liquor by dispersive solid phase extraction–gas chromatography-mass spectrometry

中文关键词:  气相色谱-质谱法  分散固相萃取  药酒  邻苯二甲酸酯

英文关键词:gas chromatography-mass spectrometry  dispersive solid phase extraction  medicinal liquor  phthalate acid ester

中文摘要:

      目的 建立气相色谱-质谱法测定药酒中15种邻苯二甲酸酯的残留量。方法 样品经60 ℃水浴蒸发乙醇后进行固相分散萃取净化, 采用DB-1701色谱柱分离; 质谱采用电子轰击离子源(electron ionization, EI)模式电离, 采用选择性离子检测(selected ion monitor, SIM)模式对15种邻苯二甲酸酯的定量离子和定性离子进行检测。比较了3种样品前处理方法对回收率的影响, 同时对空白干扰问题进行了讨论。结果 本方法在10 min内完成样品前处理, 在30 min内完成对15种目标化合物的较好分离, 15种邻苯二甲酸酯在0.5~8 mg/L范围内线性关系良好(r2 ≥0.9991), 在0.1、1.0和3.0 μg/mL 3个添加水平上的回收率为88.0%~123.7%, 相对标准偏差小于2.9 %(n=6), 检出限在0.002~0.04 mg/L之间。结论 该方法操作简单准确, 可适用于药酒中邻苯二甲酸酯的检测。

英文摘要:

      Objective To establish a method for the determination of 15 kinds of phthalate acid ester in medicinal liquor by gas chromatography-mass spectrometry (GC-MS). Method Samples were evaporated ethanol under 60 ℃ water bath, purified with dispersive solid phase extraction, and separated by DB-1701 column. Using electron ionization (EI) mode and selected ion monitor (SIM) mode, the quantitative and qualitative ions of 15 kinds of phthalate acid ester were detected by mass spectrum. Meanwhile, the effect of 3 kinds of sample preparation methods on the recovery was compared, and the problem of blank interference in this experiment was discussed. Result The method spend 10 min to complete the sample pretreatment, and spend 30 min to realize a good separation of 15 kinds of target compounds by GC-MS. Fifteen kinds of phthalate acid ester had a good linear relationship in the range of 0.5~8 mg/L with correlation coefficient r2≥0.9991. The recoveries spiked at 3 levels of 0.1, 1.0 and 3.0 μg/mL were ranged from 88.0% to 123.7% with relative standard deviations (RSD) less than 2.9% (n=6). The limits of detection was 0.002~0.04 mg/L. Conclusion The method is simple and accurate, which can be used for the determination of phthalate acid ester in medicinal liquor.