UPLC-MS/MS法测定盐酸法舒地尔注射液中高哌嗪  

Determination of Homopiperazine in Fasudil Hydrochloride Injection by UPLC-MS/MS

作　　者：邵红霞 汪辉 秦秋明 SHAO Hong-xia;WANG Hui;QIN Qiu-ming(Shanghai WeiPu Chemical Technology Service Co.,Ltd.,Shanghai 200438,China)

机构地区：[1]上海微谱化工技术服务有限公司,上海200438

出　　处：《浙江化工》2021年第7期40-44,共5页Zhejiang Chemical Industry

摘　　要：目的:建立超高效液相-串联质谱法(UPLC-MS/MS)测定盐酸法舒地尔注射液中高哌嗪含量。方法:样品用适量1 mol·L~(-1)的氢氧化钠溶液稀释后用乙腈萃取进样;流动相:甲醇-0.1%甲酸水溶液,色谱柱:ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm);电喷雾化学电离(ESI),多反应监测(multiple reaction monitoring, MRM),正离子扫描模式。结果:高哌嗪在360~2400μg·L~(-1)(相关系数r=0.9977)内表现出良好的线性关系,重复性试验的相对平均偏差(RSD)为1%,方法回收率为87%~100%,检测下限(S/N约为3)为60μg·L~(-1),溶液在室温下24 h内稳定。结论:本试验建立了盐酸法舒地尔注射液中高哌嗪的测定方法,该方法具有前处理简单、分析快速、灵敏度高、测定结果准确、专属性强等诸多优点,可应用于药物质量监测。Objective:To establish an ultra high performance liquid phase-tandem mass spectrometry(UPLC-MS/MS)method for the determination of homopiperazine in fasudil hydrochloride injection.Methods:The sample was diluted with an appropriate amount of 1 mol·L-1 sodium hydroxide solution,then extracted and injected with acetonitrile.Mobile phase:methanol-0.1%formic acid aqueous solution,column:ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm);Multiple reaction monitoring(MRM)mode was performed with Electron Spray Ionization(ESI)operating in the positive ionization mode.Results:Homopiperazine had a good linear relationship within 360~2400μg·L-1(correlation coefficient r=0.9977).The relative average deviation(RSD)of the repeatability tests was 1%,the recovery rate was 87%~100%,the LOD(S/N was about 3)was 60μg·L-1.The sample solution was stable within 24 h at room temperature.Conclusion:This experiment has established a method for the determination of homopiperazine in fasudil hydrochloride injection.This method has the advantages of simple pretreatment,rapid analysis,high sensitivity,accurate determination results,and strong specificity.It can be applied to the quality monitoring of drugs.

关 键 词：UPLC-MS/MS 高哌嗪 盐酸法舒地尔注射液 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]