QuEChERS-超高效液相色谱-串联三重四极杆质谱法同时测定猪肉中24种兽药残留

Simultaneous determination of 24 kinds of veterinary drug residues in pork by QuEChERS-ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry

中文关键词:  QuEChERS 前处理技术  超高效液相色谱-串联质谱法  基质效应 多兽药残留

英文关键词:QuEChERS  pretreatment technology  ultra performance liquid chromatography-tandem mass spectrometry  matrix effect  multiple veterinary drug residue

中文摘要:

      目的 建立QuEChERS技术结合超高效液相色谱-串联三重四极杆质谱法(ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry, UPLC-MS/MS)同时测定猪肉中24种兽药残留快速检测方法。方法 样品经0.1%甲酸乙腈溶液提取, 3 g无水MgSO4和2 g C18 E净化, Thermo-Fisher Hypersil GOLD aQ色谱柱(50 mm×2.1 mm, 1.9 μm)分离, 乙腈和0.1%甲酸水溶液梯度洗脱, 在电喷雾正离子扫描的模式下进行定性和定量的检测。结果 24种兽药线性关系良好, 相关系数均达0.9910以上, 检出限范围为0.2~10.0 μg/kg, 方法回收率范围为70.2%~110.3%, 相对标准偏差为1.2%~13.8%。结论 该方法简便、快速、准确、实用性强, 适用于猪肉中兽药残留的检测。

英文摘要:

      Objective To establish a rapid detection method for the simultaneous determination of 24 kinds of veterinary drug residues in pork by QuEChERS technique combined with ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with acidified acetonitrile, salted out by 3 g magnesium sulfate anhydrous and 2 g C18 E, separated by Thermo-Fisher Hypersil GOLD aQ chromatographic column (50 mm×2.1 mm, 1.9 μm) via gradient elution of acetonitrile and 0.1% formic acid aqueous solution. The gradient elution of acetonitrile and 0.1% formic acid in aqueous solution was performed in the mode of electrospray positive ion scanning. Results The linear relationship of 24 kinds of veterinary drugs was good, and the correlation coefficients were greater than 0.9910, and the detection limit ranged from 0.2–10.0 μg/kg. The spiked recoveries varied between 70.2%–110.3%, and the relative standard deviations were 1.2%–13.8%. Conclusion The method is simple, rapid, accurate, practical, and suitable for detection of multiple veterinary drug residues in pork.