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,2μm)分离,以5 mmol/L乙酸铵缓冲溶液(p H 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0.08~1.0μg/g、0.1~2.5μg/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。
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,2μm),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 0.08~1.0μg/g and the limits of quantitation(LOQs)were0.1~2.5μg/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.
作者
具笑平
陈腾辉
吴芳花
吴志国
Ju Xiaoping;Chen Tenghui;Wu Fanghua;Wu Zhiguo(Heyuan Institute of Drug Control,Heyuan 517025,China)
出处
《广东化工》
CAS
2024年第7期139-142,131,共5页
Guangdong Chemical Industry
