吹扫捕集-气相色谱-三重四极杆串联质谱法测定水产品中苯系物残留

Determination of benzeneseries residues in aquatic products by purge-and-trap and gas chromatography-triple quadrupole mass spectrometry

中文关键词:  吹扫捕集  气相色谱-三重四极杆串联质谱法  水产品  苯系物

英文关键词:purge-and-trap  gas chromatography-triple quadrupole mass spectrometry  aquatic products  benzene series

中文摘要:

      目的 建立一种适用于水产品中7种苯系物残留检测的吹扫捕集-气相色谱-三重四极杆串联质谱法。方法 样品采用吹扫捕集技术, 在25 ℃的吹扫温度下以40 mL/min的吹扫流速将目标物富集后导入HP-INNOWax (30 m×250 μm, 0.25 μm)极性毛细管色谱柱进行分离, 气相色谱-串联质谱的多反应监测(multiple reaction monitoring, MRM)模式测定, 通过将待测目标物保留时间及特征离子与标准质谱图相比较进行定性, 采用氟苯作为内标进行定量。结果 7种苯系物的响应值与其质量浓度在0.5~50.0 ng/mL范围内的线性关系良好, 相关系数均大于0.9954; 在2.0~40.0 μg/kg添加浓度下, 鲈鱼、对虾和牡蛎样品的日内和日间加标回收实验平均回收率为73.9%~103.0%, 相对标准偏差为2.26%~11.60%; 检出限为1.0 μg/kg, 定量限为2.0 μg/kg。结论 该方法灵敏度高、稳定性好, 适用于水产品中7种苯系物残留的检测。

英文摘要:

      Objective To establish a suitable method for the detection of 7 kinds of benzene series residues in aquatic products by purge-and-trap and gas chromatography-triple quadrupole mass spectrometry. Methods The purge and trap technology was adopted for the samples, the target substance was enriched at the purge temperature of 25 ℃ and the purge flow rate of 40 mL/min before being introduced into an HP-INNOWax (30 m×250 μm, 0.25 μm) polar capillary column for separation, multiple reaction monitoring (MRM) mode of gas chromatography-tandem mass spectrometry was used for determination, the retention time and characteristic ions of the target substance to be tested were compared with the standard mass spectrum for qualitative analysis, and fluorobenzene was used as the internal standard for quantitative analysis. Results The linear relationships between the response values of the 7 kinds of benzene series compounds and their mass concentrations in the range of 0.5?50.0 ng/mL were good, and the correlation coefficients were all greater than 0.9954; at the concentration of 2.0?40.0 μg/kg, the average recoveries of weever, prawn and oyster samples spiked in the daytime and in the daytime were 73.9%?103.0%, and the relative standard deviations were 2.26%?11.60%. The limit of detection was 1.0 μg/kg and the limit of quantitation was 2.0 μg/kg. Conclusion This method has high sensitivity and good stability, and is suitable for the determination of 7 kinds of benzene series residues in aquatic products.