固相萃取-超高效液相色谱-串联质谱法测定禽蛋中的67种禁用药物

Determination of 67 kinds of prohibited drugs in poultry eggs by solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  固相萃取  禁用药物  禽蛋产品

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  prohibited drugs  poultry egg products

中文摘要:

      目的 建立固相萃取-超高效液相色谱-三重四极杆串联质谱法(solid phase extraction-ultra performance liquid chromatography-triple quadrupole-tandem mass spectrometry, SPE-UPLC-QqQ-MS/MS)测定禽蛋中的67种禁用药物残留的分析方法。方法 样品用Mcllvaine-Na2EDTA缓冲溶液提取, 加入钨酸钠沉淀蛋白, 经Anavo HLB固相萃取柱净化后采用ACQUITY UPLC HSS T3柱(100 mm×2.1 mm, 1.8 μm)分离, 正离子模式以0.1%甲酸水溶液-甲醇为流动相、负离子模式以水-乙腈为流动相进行梯度洗脱, 在UPLC-QqQ-MS/MS多反应监测模式下进行定性定量分析, 同位素内标法或基质匹配外标法定量。结果 67种禁用药物在0.1~100.0 μg/kg范围内均呈现良好的线性关系, 相关系数r2≥0.99, 方法的定量限范围为0.1~0.5 μg/kg。平均加标回收率为56.3%~110.1%, 相对标准偏差为1.5%~16.8%。结论 本方法操作简单、准确性高、成本较低, 可实现禽蛋中禁用药物残留的高通量分析。

英文摘要:

      Objective To establish an analytical method for the determination of 67 kinds of prohibited drug residues in poultry eggs by solid phase extraction-ultra performance liquid chromatography-triple quadrupole-tandem mass spectrometry (SPE-UPLC-QqQ-MS/MS). Methods The samples were extracted with Mcllvaine-Na2EDTA buffer solution and the proteins were precipitated with sodium tungstate. The separation was performed on an ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) after cleanup with by Anavo HLB solid phase extraction column. The gradient elution was performed in positive ion mode using 0.1% formic acid aqueous solution-methanol as mobile phase and in negative ion mode using water-acetonitrile as mobile phase. Qualitative and quantitative analysis was performed in UPLC-QqQ-MS/MS multiple reaction monitoring mode, and quantitative analysis was performed by isotope internal standard method or matrix matching external standard method. Results The 67 kinds of prohibited drugs showed good linearity in the range of 0.1?100.0 μg/kg with the correlation coefficients r2≥0.99, and the limits of quantification were in the range of 0.1?0.5 μg/kg. The average recoveries of the spiked samples were 56.3%?110.1% with the relative standard deviations of 1.5%?16.8%. Conclusion This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs with a simple, accurate, low-cost procedure.