UPLC-MS/MS检测女金丸中9种青霉素类抗生素残留  

Detection of 9 Penicillin Antibiotics Residues in Nujin pill by UPLC-MS/MS

作　　者：李应才 黄合琤 董丽荣 杨野[2] LI Yingcai;HUANG Hecheng;DONG Lirong;YANG Ye(Kunming Institute for Food and Drug Control,Kunming,650032,China;Kunming University of Science and Technology,Kunming,650500,China)

机构地区：[1]昆明市食品药品检验所,云南昆明650032 [2]昆明理工大学,云南昆明650500

出　　处：《云南中医学院学报》2022年第1期79-83,共5页Journal of Yunnan University of Traditional Chinese Medicine

基　　金：云南省科技厅项目(云南省青年拔尖人才YNWR-QNBJ-2019-124)。

摘　　要：目的建立超高效液相色谱-串联质谱法同时检测女金丸中9种青霉素类抗生素残留。方法采用ACQUITY UPLC BEH-C18色谱柱(2.1 mm×50 mm,1.7μm)分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱。在电喷雾离子源,正离子模式下,以多反应监测模式(MRM)扫描进行检测,外标法定量。结果9种抗生素在相应范围内呈良好线性关系,相关系数(r)均大于0.999;检测限为0.01~0.03 ng·mL^(-1),定量限为0.02~0.1 ng·mL^(-1);平均回收率(n=6)为75.4%~100.2%,RSD为0.54%~3.43%。结论该方法准确、简便、灵敏、高效,可用于女金丸中9种青霉素类抗生素残留的检测。Objective To develop a method based on ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the simultaneous determination of nine penicillin antibiotics residues in Nujin pill.Methods The samples were separated on the CQUITY UPLC BEH-C18(2.1 mm×50 mm,1.7μm)chromatographic column by gradient elution using 0.1%formic acid andacetonitrle as the mobile phase.The electrospray ion source was operated in the positive ion mode using the multi-reaction monitoring(MRM)methed,and the results were quantified by the external standard method.Results The correlation coefficients(r)of the nine drugs were all greater than 0.999 in the corresponding mass concentrationranges,and the detection limit was 0.01~0.03 ng·m L^(-1) and the quantitative limit was 0.02~0.1 ng·m L^(-1).The average recovery(n=6)was 75.4%~100.2%and RSD was 0.54%~3.43%.Of the 30 samples tested,1 was found to contain dicloxacillin at a level of 0.193 mg·kg^(-1).No other drugs were found.Conclusion The method is accurate,simple,sensitive and highly effective.It can be used for the determination of nine kinds of penicillin residues in traditional Chinese medicine pills.

关 键 词：高效液相色谱-串联质谱 女金丸 青霉素 双氯西林 

分 类 号：R286.0[医药卫生—中药学]