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
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
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。
ObjectiveTo 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). MethodsThe 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. ResultsThe 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. ConclusionThis method is simple and sensitive, and can meet the monitoring needs of nitroimidazoles in traditional Chinese veterinary medicine.
标题：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
英文标题：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
作者：
马东杰 华北制药金坦生物技术股份有限公司
艾连峰 石家庄海关技术中心
霍惠玲 河北省兽药监察所
王敬 石家庄海关技术中心
李研东 河北省兽药监察所
张海超 石家庄海关技术中心
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,
发表日期：2020-03-13
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