固相萃取-液相色谱-串联质谱法快速测定猪肉中27种兽药及代谢物残留量

Simultaneous determination of 27 kinds of veterinary drugs and their metabolites in swine meat by liquid chromatography-tandem mass spectrometry with solid phase extraction

中文关键词:  猪肉  磺胺类药物  喹诺酮类药物  苯并咪唑类药物  通过型固相萃取  液相色谱-串联质谱法

英文关键词:swine meat  sulfonamides  quinolones  benzimidazoles  pass-through solid phase extraction  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立了固相萃取-液相色谱-串联质谱法快速测定猪肉中27种兽药(磺胺类、喹诺酮类及苯并咪唑类药物)及代谢物残留量的分析方法。方法 匀质后的猪肉样品用80%乙腈溶液提取，提取后用EMR-Lipid固相萃取小柱净化，流出液直接进行上机测定，采用ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm，1.8 μm)分离，以0.1%甲酸溶液（含5 mmol/L乙酸铵）和乙腈作为流动相进行梯度洗脱，电喷雾正离子模式下监测，内标法定量。结果 27种化合物在0.075～50 μg/L范围内线性关系良好，相关系数(r2)均高于0.9980，方法检出限和定量限分别在0.06~0.3 μg/kg和0.2~1.0 μg/kg范围之间。27种兽药及代谢物在1、10和100 μg/kg添加浓度水平下平均添加回收率在88.5%~104%之间，相对标准偏差在2.6%~8.0%之间。结论 该方法准确度和灵敏度高，前处理简单快速，适用于猪肉中磺胺类药物、喹诺酮类药物及苯并咪唑类药物的同时分析。

英文摘要:

      Objective To establish a simple and fast analytical method for simultaneous determination of residues of 27 kinds of veterinary drugs (sulfonamides, quinolones, and benzimidazoles) and their metabolites in swine meat by liquid chromatography-tandem mass spectrometry with solid phase extraction. Methods The homogenized meat samples were extracted with 80% acetonitrile solution. After extraction, a solid phase extraction procedure was carried out with EMR-lipid cartridge without activation procedure. Then, the effluent was collected and directly used for chromatographic separation on an ACQUITY UPLC HSS T3 column with a gradient elution of 0.1% formic acid in water with 5 mmol/L ammonium acetate/acetonitrile. The compounds were monitored in positive ion mode using multiple reaction monitoring mass spectrometry and quantified by internal standard method. Results Good linear relationship had been obtained ranging from 0.075 to 50 μg/L for the 27 veterinary drugs and their metabolites, and the correlation coefficients (r2) were higher than 0.9980. Excellent Limits of detection (0.06~0.30 μg/kg) and limits of quantification (0.20~1.0 μg/kg) had been obtained. The average recoveries varied from 88.5 to 104 % at 1, 10 and 100 μg/kg fortification level. Moreover, all of relative standard deviations were less than 8%. Conclusion The method has high accuracy and sensitivity, simple and fast pre-treatment, and is suitable for the simultaneous analysis of sulfonamides, quinolones, and benzimidazoles in swine meat.