超高效液相色谱-串联质谱法快速测定妥曲珠利等兽药在液态乳中的残留

Rapid determination of toltrazuril and other veterinary drug residues in milk by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  液态乳  抗球虫药  固相萃取  超高效液相色谱-串联质谱法  快速测定

英文关键词:milk  coccidiostat  solid-phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  rapid determination

中文摘要:

      目的 建立基于超高效液相色谱-串联质谱法, 结合通过式固相萃取净化技术快速检测妥曲珠利等兽药在液态乳中残留量的方法。方法 样品经0.1%乙酸乙腈溶液超声提取后, 选用通过式固相萃取柱(HMR-Lipid)净化, 以0.1?乙酸水-乙腈为流动相在BEH C18色谱柱中分离, 目标物在电喷雾负离子模式下电离, 多反应监测模式下检测和分析, 内标法定量。对样品中目标物的提取、净化、色谱条件等关键因素进行了优化。结果 各目标物在0.5~50.0 ng/mL的质量浓度范围内线性良好, 相关系数均的大于0.999, 检出限为0.23~0.52 μg/kg, 定量限为0.23~1.45 μg/kg, 加标回收率在92.4%~105.2%, 精密度在0.32%~7.00%。结论 该方法实验前处理可控制在15 min内完成, 操作简便、快速、灵敏度高、定性定量准确, 适用于液态乳中妥曲珠利等抗球虫药物残留的快速检测。

英文摘要:

      Objective To establish a method for rapid detection of toltrazuril and other veterinary drug residues in milk using ultra performance liquid chromatography-tandem mass spectrometry based on solid-phase extraction purification technology. Methods The samples were ultrasonically extracted with a 0.1% acetic acid-acetonitrile solution and purified using an solid phase extraction column (HMR-Lipid). Separation was achieved on a BEH C18 chromatographic column with 0.1? acetic acid in water-acetonitrile as the mobile phase. The target compounds were ionized in the negative ion mode of electrospray ionization and detected in multiple reaction monitoring mode, with quantification performed using the internal standard method. Factors such as extraction, purification and chromatographic conditions of the target compounds in the samples were optimized. Results The target compounds had good linearity in the mass concentration range of 0.5–50.0 ng/mL, with correlation coefficients all greater than 0.999. The limits of detection were 0.23–0.52 μg/kg, and the limits of quantitation were 0.23–1.45 μg/kg. The spiked recoveries ranged from 92.4% to 105.2%, and the precisions were between 0.32% and 7.00%. Conclusion The sample pretreatment could be completed within 15 minutes. This method is simple, rapid, highly sensitive and accurate for both qualitative and quantitative analysis, and is suitable for the detection of toltrazuril and other veterinary drug residues in milk.