UPLC-MS/MS法测定注射用伏立康唑产品工艺组件中2,5-二甲基-2,5-己二醇  

Determination of 2,5-Dimethyl-2,5-hexanediol in Process Components of Voriconazole Products for Injection by UPLC-MS/MS

作　　者：汪辉 邵红霞 秦秋明 WANG Hui;SHAO Hong-xia;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8期43-48,共6页Zhejiang Chemical Industry

摘　　要：目的:建立超高效液相-串联质谱法(UPLC-MS/MS)测定注射用伏立康唑产品工艺组件中2,5-二甲基-2,5-己二醇(DHD)的方法。方法:样品用水复溶后加入内标2-甲基戊烷-2,4-二醇(MPD),用乙腈萃取后进样。采用液质联用仪进行分析,流动相A为甲醇,流动相B为0.1%氨水溶液;利用柱ACQUITY UPLC BEH PHENYL(2.1 mm×50 mm,1.7μm)分离;采用电喷雾电离源、多反应监测(multiple reaction monitoring,MRM)模式对待测物进行负离子扫描检测。结果:DHD在10.0~68.0μg·L-1(r=0.9990)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84%~107%,方法检测下限(S/N≈3)为3.3 ppb,定量下限(S/N≈10)为10.0 ppb,溶液在室温下24 h内稳定。结论:UPLC-MS/MS法具有灵敏度高、测定结果准确、专属性强等诸多优点,可用于注射用伏立康唑工艺组件中DHD的风险监测,亦可为其他类产品中DHD的检测提供参考。Objective:To establish an utral high performance liquid phase-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 2,5-dimethyl-2,5-hexanediol(DHD)in process components of voriconazole for injection.Methods:The sample was redissolved by water and added with internal standard 2-methylpentane-2,4-diol(MPD),extracted with acetonitrile and injected.The liquid mass spectrometer was used for analysis.The mobile phase A was methanol,and mobile phase B was 0.1%ammonia solution.Column ACQUITY UPLC BEH PHENYL(2.1 mm×50 mm,1.7μm)was used for separation.Electrospray ionization source and multiple reaction monitoring(MRM)mode were used for negative ion scanning detection.Results:DHD shows a good linearity within between 10.0~68.0μg·L-1(r=0.9990).The relative average deviation(RSD)of repeatability test is 1%,and the method recovery rate is 84%~107%.The lower limit of detection(S/N≈3)is 3.3 ppb,and the lower limit of quantification(S/N≈10)is 10.0 ppb.The sample solution is stable in 24 h at room temperature.Conclusion:UPLC-MS/MS method has many advantages,such as high sensitivity,accurate determination results,strong specificity and so on.It can be applied to the risk monitoring of DHD in process components of voriconazole for injection,and can provide a reference for the detection of DHD in other products.

关 键 词：UPLC-MS/MS 2 5-二甲基-2 5-己二醇 工艺组件 伏立康唑 

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