摘要
目的建立测定甲状腺片中7种喹诺酮类药物残留的高效液相色谱-质谱/质谱(LC-MS/MS)方法。方法ACQUITY UPLC?^(■)BEH C18(2.1 mm×100 mm,1.7μm)为色谱柱,乙腈为流动相A、0.1%甲酸为流动相B梯度洗脱,流速为0.3 mL/min,柱温为40℃,采用LC-MS/MS法,电喷雾离子源,多反应监测模式,正离子扫描方式进行检测。结果7种喹诺酮类药物在1~100 ng/mL浓度范围内线性关系良好。7种喹诺酮类药物平均加样回收率均在85.0%~100.0%范围内,RSD均小于3.5%。结论所建方法灵敏度高、准确,结果稳定、杂质干扰小、特异性强,可用于甲状腺片中喹诺酮类药物残留的检测。
Objective To establish a high performance liquid chromatography-mass spectrometry/mass spectrometry(LC-MS/MS)method for the determination of seven quinolones residues in Thyroid Tablets.Methods The column was ACQUITY UPLC^(■)BEH C18(2.1 mm×100 mm,1.7μm).Acetonitrile was used as mobile phase A and 0.1%formic acid as mobile phase B for gradient elution.The flow rate was 0.3 mL/min,the column temperature was 40℃.LC-MS/MS method,electrospray ionization source,multiple reaction monitoring and positive ion scanning method were used for detection.Results Seven quinolones showed good linear relationship in the concentration range of 1-100 ng/mL.The average recoveries of seven kinds of quinolones were in the range of 85.0%-100.0%,and RSDs were all less than 3.5%.Conclusion The established method is sensitive,accurate,stable,with little interference from impurities and strong specificity.It can be used for the determination of quinolone residues in Thyroid Tablets.
作者
赵文法
王春雷
冯家龙
ZHAO Wenfa;WANG Chunlei;FENG Jialong(Liaocheng Institute for Food and Drug Control,Shandong Province,Liaocheng252000,China)
出处
《中国医药导报》
CAS
2021年第9期20-23,共4页
China Medical Herald
基金
山东省药品质量风险监测项目(鲁药监办﹝2019﹞14号-23)。
关键词
甲状腺片
喹诺酮类
药物残留
液相色谱-质谱
Thyroid Tablets
Quinolones
Drug residue
Liquid chromatography-mass spectrometry