高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量

Determination of benzimidazoles and its metabolites residues in dairy and dairy products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  苯并咪唑类药物及其代谢物  高效液相色谱-串联质谱  乳制品

英文关键词:benzimidazoles and its metabolites  high performance liquid chromatography-tandem mass  dairy products

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量的方法。方法 样品采用水-乙腈溶液提取, 氯化钠盐析, 饱和正己烷脱脂净化直接稀释后, 经Atlantis T3 (4.6 mm×100 mm, 3 μm)色谱柱分离, 以乙腈-0.1%甲酸溶液为流动相, 采用电喷雾离子源质谱, 在正离子扫描方式下以多反应监测(multiple response monitoring, MRM)模式检测, 外标法定量。结果 19种苯并咪唑类药物及其代谢物在3个加标水平下的平均回收率为70.7%~110.0%, 相对标准偏差为2.3%~9.9%。在0.2~10 μg/L质量浓度范围内线性关系良好, 定量限为10~80 μg/kg。结论 该方法操作简便, 灵敏度高, 抗干扰能力强, 回收率和重复性良好, 适用于乳和乳制品中苯并咪唑类药物及其代谢物的测定。

英文摘要:

      Objective To establish a method of determination of benzimidazoles and its metabolites residues in dairy and dairy products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with acetonitrile-water, then salted out by sodium chloride and degreased by hexane. The targeted compounds were separated with a Atlantis T3(4.6 mm×100 mm, 3 μm) with the mobile phases of acetonitrile and 0.1% formic acid and detected by electrospray ionization mass spectrometry in positive and multiple reaction monitoring (MRM) mode. The quantification was performed by the external standard method. Results The recoveries at the 3 spiked levels were in the range of 70.7%?110.0% with the relative standard deviations in the range of 2.3%?9.9%. The calibration curves showed good linearity in the range of 0.2?10 μg/L. The limits of quantification were 10?80 μg/kg. Conclusion This method is easy to operate, it has high sensitivity, strong anti-interference ability, good recovery and repeatability, which is suitable for the determination of benzimidazole drugs and their metabolites in milk and dairy products.