液相色谱串联质谱法同时测定消毒产品中抗感染药物
Simultaneous Determination of Anti-infective Drugs in Disinfection Products by HPLC-MS/MS
具笑平 1陈腾辉 1吴芳花 1吴志国1
作者信息
- 1. 河源市药品检验所,广东 河源 517025
- 折叠
摘要
目的:建立HPLC-MS/MS同时检测消毒产品中非法添加33种抗感染药物的方法.方法:样品经过乙腈(含0.5%甲酸)超声提取,采用Shim-pack GIST C18色谱柱(2.1 mm×100 mm,2 μm)分离,以5 mmol/L乙酸铵缓冲溶液(pH 4.0)-乙腈(含 0.1%甲酸)为流动相,梯度洗脱,流速为0.3 mL/min-1,柱温40℃;采用电喷雾离子源(ESI)正、负离子模式,多反应监测(MRM)模式进行检测.通过比较分子离子峰、二级碎片离子峰、色谱保留时间等确定添加的药物.结果:在10～100 ng/mL的线性范围内,所检测的 33种抗感染药物相关系数(r)均大于 0.99,线性关系良好,该方法的检出限和定量下限分别为 0.08～1.0 μg/g、0.1～2.5 μg/g.平均加样回收率为 80.0%～118.0%,RSD为0.1%～3.8%;精密度、重复性试验的RSD在0.66%～11.85%.结论:经方法学验证,所建立的分析方法可靠、灵敏、简便,降低假阴性、假阳性风险,可用于快速检测消毒产品中非法抗感染的药物.
Abstract
Objective:To establish an HPLC-MS/MS method for simultaneous of anti-infective drugs illegally added in disinfection Products.Methods:The samples were extracted with acetonitrile(containing 5%formic acid).The analysis was performed on Shim-pack GIST C 18 column(2.1 mm×100 mm,2 μm),the mobile phase was 5 mmol/L ammonium acetate pH 4.0-0.1%formic acid in acetonitrile solution with gradient elution,and flow rate was 0.3mL/min and the column temperature was 40℃.Mass spectrometry acquisition was done in positive,negative ion mode with electrospray ionization mode(ESI)and analyses were detected in MRM mode.The chemical drugs were determined by comparing the molecular ion peaks,the second-order fragment ion peaks,the chromatographic retention time,and the content of the added drugs was calculated by theexternal standard method based on the peak area of the mass spectrum.Results:indicated that in the range of 10～100 ng/mL,the present method showed good linear trend with the correlation coefficients(r)all above 0.99.The limits of detection(LODs)were 0.08～1.0 μg/g and the limits of quantitation(LOQs)were0.1～2.5 μg/g.and the average recoveries were in the range of 80.0%～118.0%with RSD of 0.1%～3.8%.The RSD of precision and repeatability were 0.66～11.85.0%.Conclusion:The method is simple,accurate with high sensitivity,which can be used to quickly detect 33 kinds of anti-infective drugs illegally added in Disinfection Product at the same time.
关键词
高效液相色谱-串联质谱(HPLC-LCMS/MS)/消毒产品/抗感染药物/非法添加Key words
HPLC-MS/MS/anti-infective drugs/disinfection product number/illegal addition引用本文复制引用
出版年
2024
NETL
NSTL
万方数据