超高效液相色谱-串联质谱法同时测定水产制品中22种全氟烷基物质

Simultaneous determination of 22 kinds of perfluorinated alkyl substances in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  水产制品  全氟烷基物质

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  aquatic products  perfluorinated alkyl substances

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时检测水产制品中22种全氟烷基物质(perfluorinated alkyl substances, PFASs)定性定量检测方法。方法 选取基质成分复杂的水产制品作为检测目标。样品经乙腈(含1%甲酸)提取液涡旋振荡提取, 分散固相萃取结合通过式固相萃取柱进行净化, C18色谱柱分离, 甲醇和5 mmol/L乙酸铵溶液梯度洗脱, 多反应监测负离子模式采集, 同位素内标法定量。结果 22种PFASs在其相应的质量浓度范围内线性关系良好, 相关系数大于0.994, 定量限为0.10~0.25 μg/kg。两种样品中添加定量限、1.0 μg/kg和 10.0 μg/kg浓度水平时平均回收率在71.8%~98.2%之间, 相对标准偏差为3.9%~10.9%。结论 该方法抗干扰性强、前处理操作简便、分析速度快、灵敏度高, 适用于水产制品中22种PFASs的快速精确检测。

英文摘要:

      Objective To establish a qualitative and quantitative method for the simultaneous determination of 22 kinds of perfluorinated alkyl substances (PFASs) in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry. Methods Aquatic products with complex matrix components were selected as the detection target. The samples were extracted by vortex oscillation from 1% formic acid-acetonitrile extract, the disper solid phase extraction was combined with purification through a type solid phase extraction column, the samples were separated by a C18 column, and then eluted by gradient elution with methanol and 5 mmol/L ammonium acetate solution, the samples were collected by multiple reaction monitoring negative ion mode, and quantified by isotope internal standard method. Results The linear relationships of the 22 kinds of PFASs were good within the corresponding mass concentrations, with the correlation coefficients greater than 0.994 and the limits of quantification were 0.10-0.25 μg/kg. The recoveries of 2 kinds of samples at spiked levels (the limit of detection, 1.0 μg/kg, 10.0 μg/kg) were 71.8%?98.2%, the relative standard deviations were 3.9%-10.9%. Conclusion This method has the advantages of strong anti-interference, simple pretreatment operation, fast analysis speed and high sensitivity, and is suitable for the rapid and accurate detection of 22 kinds of PFASs in aquatic products.