摘要
采用超高效液相色谱-串联三重四极杆质谱(UPLC-MS/MS)技术,建立了动物源性中药鸡内金中磺胺甲𫫇唑等9种磺胺类药物残留的检测方法。样品经QuEChERS法提取,离心后上清液经PRiME HLB固相萃取柱净化,采用ACQUITY BEH C_(18)柱(2.1 mm×100 mm,1.7μm)分离,以含0.1%甲酸-2 mmol/L乙酸铵的水溶液和含0.1%甲酸的乙腈溶液为流动相进行梯度洗脱,在电喷雾正离子模式下,以动态多反应监测模式(d-MRM)进行检测,外标法定量。结果表明9种磺胺类药物在0~50 ng/mL范围内呈良好的线性关系,相关系数(r^(2))均不小于0.9960,方法检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.0654~0.7157μg/kg和0.2122~2.478μg/kg;在3个加标水平下的回收率为63.2%~88.7%,相对标准偏差(RSD)为0.90%~7.1%。该方法简单、快速、准确,应用该方法筛查10批鸡内金样品,有1批检出磺胺甲𫫇唑残留。
In order to evaluate the risk of sulfonamides residues in Gizzard Pepsin,a comprehensive analytical method was developed for the qualitative and quantitative determination of nine kinds of sul⁃fonamides in Gizzard Pepsin by ultra-performance liquid chromatography coupled with triple quadru⁃pole mass spectrometry(UPLC-MS/MS)in this paper.The sample was extracted by QuEChERS with ultrasonic method,then purified with PRiME HLB.The chromatographic separation was performed on an ACQUITY BEH C_(18) chromatographic column(2.1 mm×100 mm,1.7μm),with 0.1%for⁃mic acid-2 mmol/L ammonium acetate aqueous solution and acetonitrile containing 0.1%formic ac⁃id as mobile phases by gradient elution.The analytes were detected by electrospray ionization mass spectrometry in positive mode under dynamic multiple reaction monitoring(d-MRM)mode,and quantified by external standard method.Results showed that the nine sulfonamides showed good lin⁃earities in the concentration range of 0-50 ng/mL with their correlation coefficients(r^(2))not less than 0.9960.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)were in the ranges of 0.0654-0.7157μg/kg and 0.2122-2.478μg/kg,respectively.The recoveries for the analytes at three spiked levels were in the range of 63.2%-88.7%,with relative standard deviations(RSD)of 0.90%-7.1%.The developed method was simple,rapid and accurate,and was applied to the detection on 10 batches of Gizzard Pepsin samples,among which one was found to con⁃tain sulfamethoxazole residue.
作者
许晓辉
王小乔
董蔚
吴福祥
杜锐浒
朱仁愿
石晓峰
XU Xiao-hui;WANG Xiao-qiao;DONG Wei;WU Fu-xiang;DU Rui-hu;ZHU Ren-yuan;SHI Xiao-feng(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China;Gansu Provincial Academic Institute for Medical Research,Lanzhou 730050,China;Lanzhou Zhongjianke Testing Technology Co.,Ltd,Lanzhou 730070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2021年第10期1497-1502,共6页
Journal of Instrumental Analysis
基金
甘肃省药品监督管理局科学技术类项目(2020GSMPA032)。
作者简介
通讯作者:石晓峰,主任药师,研究方向:天然药物化学与中药质量标准,E-mail:shixiaofeng2005@sina.com。
