通过式固相萃取-超高效液相色谱串联质谱法快速测定中兽药制剂中４种硝基咪唑类药物

Rapid and simultaneous determination of 4 nitroimidazoles in traditional Chinese veterinary medicine by pass-through solid phase extraction purification and ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  通过式固相萃取  超高效液相色谱串联质谱法  中兽药制剂  硝基咪唑类药物

英文关键词:pass-through solid phase extraction  ultra performance liquid chromatography tandem mass spectrometry  traditional Chinese veterinary medicine  nitroimidazoles

中文摘要:

      目的 建立通过式固相萃取-超高效液相色谱串联质谱法(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)同时快速测定中兽药制剂中4种硝基咪唑类药物的方法。方法 样品(2.0 g)经乙醇超声提取, 采用PRiME HLB固相萃取柱净化, 以0.1%甲酸溶液和乙腈为流动相, ACQUITY BEH C18色谱柱分离, 电喷雾正离子扫描, 多反应监测模式进行液相色谱串联质谱检测。结果 4种目标化合物在1~100 ng/mL范围内线性良好, 相关系数r2>0.999。在3个加标水平(25、50和250 μg/kg)下, 4种化合物的平均回收率范围为70.0%~93.8%, 相对标准偏差范围为1.2%~13.0%。方法的检出限为10 μg/kg; 定量限为 25 μg/kg。结论 该方法操作简便、灵敏度高, 可满足中兽药制剂中硝基咪唑类药物的监测需求。

英文摘要:

      Objective To establish a method for the rapid and simultaneous determination of 4 nitroimidazoles in traditional Chinese veterinary medicine by pass-through solid phase extraction (SPE) purification with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods The samples (2.0 g) were extracted by ethanol, and then cleaned up with an Oasis PRiME HLB pass-through SPE column. The analytes were separated on a C18 reversed-phase column with 0.1% (V/V) formic acid aqueous solution and acetonitrile as mobile phases and finally analyzed using electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM) for determination by LC-MS/MS. Results The linear ranges of the 4 compounds were from 1 to 100 ng/mL with the correlation coefficients (r2) more than 0.999. The average recoveries and relative standard deviations were 70.0%-93.8% and 1.2%-13.0% respectively at 3 spiked levels (25, 50 and 250 μg/kg). The limits of detection and the limits of quantification were 10 μg/kg and 25 μg/kg respectively for the 4 nitroimidazoles. Conclusion This method is simple and sensitive, and can meet the monitoring needs of nitroimidazoles in traditional Chinese veterinary medicine.