全自动固相萃取-超高效液相色谱-串联质谱法测定水产品中10类30种农兽药残留

Determination of 10 class and 30 kinds of pesticide and veterinary drugs residues in aquatic products by automated solid-phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  水产品  农药残留 兽药残留  全自动固相萃取-液相色谱-串联质谱

英文关键词:aquatic products  pesticide residues  veterinary drug residues  automated solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立全自动固相萃取-超高效液相色谱-串联质谱法同时测定水产品中磺胺类、四环素类、喹诺酮类、大环内酯类、硝基咪唑类、三苯甲烷类、β-内酰胺类、激素类、有机磷类、氨基甲酸酯类10类30种农兽药残留量的方法。方法 样品用甲酸乙腈溶液提取后, 使用HLB固相萃取小柱净化, 以0.1%甲酸乙腈-0.1%甲酸水为流动相, Waters ACQUITY UPLC BEH C18色谱柱分离, 使用SCIEX\Triple Quad 5500+串联三重四级杆质谱仪进行分析检测。结果 30种化合物在质量浓度为5~100 μg/L范围内的线性关系良好, 相关系数在0.9914~0.9998之间, 检出限均小于等于0.025 mg/kg, 定量限均小于等于0.050 mg/kg。样品平均回收率为62.8%~108.1%, 相对标准偏差为1.0%~14.7% (n=6)。结论 该方法精密度高、准确性好、操作自动化程度高, 可用于水产品中农兽药残留的高通量检测。

英文摘要:

      Objective To develop a method for the simultaneous determination of 30 kinds of pesticide and veterinary drug residues across 10 classes-including sulfonamides, tetracyclines, quinolones, macrolides, nitroimidazoles, triphenylmethanes, β-lactams, hormones, organophosphorus compounds and carbamates in aquatic products by automated solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry. Methods Samples were extracted with acetonitrile containing formic acid, purified using HLB solid-phase extraction cartridges, and separated on a Waters ACQUITY UPLC BEH C18 column with a mobile phase consisting of 0.1% formic acid in acetonitrile and 0.1% formic acid in water, and analyzed by a SCIEX\Triple Quad 5500+ tandem mass spectrometer. Results The 30 kinds of compounds exhibited good linearity within the concentration range of 5–100 μg/L, with correlation coefficients ranging from 0.9914 to 0.9998. The limits of detection were less than or equal to 0.025 mg/kg, and the limits of quantitation were less than or equal to 0.050 mg/kg. Mean recoveries for spiked samples ranged from 62.8% to 108.1%, with relative standard deviations of 1.0%–14.7% (n=6). Conclusion The method demonstrates high precision, good accuracy and a high degree of automation, making it suitable for high-throughput screening of pesticide and veterinary drug residues in aquatic products.