盐酸吡格列酮片中3-硝基吡咯和硫脲的定性定量方法研究  

Study on Qualitative and Quantitative Methods of 3-nitropyrrole and Thiourea in Pioglitazone Hydrochloride Tablets

作　　者：吴月霞 朱艳春 陈杰 WU Yue-xia;ZHU Yan-chun;CHEN Jie(Henan Institute for Drug and Medical Device Inspection(Henan Vaccine Issuance Center),Henan Zhengzhou 450018,China)

机构地区：[1]河南省药品医疗器械检验院(河南省疫苗批签中心),河南郑州450018

出　　处：《中国药物评价》2024年第2期101-104,共4页Chinese Journal of Drug Evaluation

摘　　要：目的:建立盐酸吡格列酮片中3-硝基吡咯和硫脲的UPLC-MS/MS定性定量方法。方法:采用Waters Cortecs T3(2.1 mm×100 mm,2.7μm)色谱柱;流动相A为0.1%甲酸(V:V)水溶液,流动相B为0.1%甲酸(V:V)乙腈溶液;梯度洗脱;柱温30℃;进样量2μL;质谱采用ESI源,正离子模式,多反应监测,对3-硝基吡咯和硫脲进行定性定量分析。结果:3-硝基吡咯和硫脲均在0.03~0.3μg·mL^(-1)范围内与峰面积线性关系良好(r>0.9995);平均加标回收率为99.06%~100.26%,RSD为0.02%~0.46%。检测限分别为0.0693~0.1407 ng·mL^(-1),定量限分别为0.2309~0.4690 ng·mL^(-1)。UPLC-MS/MS法可以对3-硝基吡咯和硫脲进行快速定性定量筛查。结论:该方法操作简单、灵敏便捷,结果准确,分析时间短至6 min,可用于盐酸吡格列酮片中3-硝基吡咯和硫脲的定性鉴别及定量检查。Objective:Oestablish a UPLC-MS/MS method for qualitative and quantitative determination of 3-nitropyrrole and thiourea in pioglitazone hydrochloride tablets.Methods:Waters Cortecs T3(2.1 mm×100 mm,2.7μm)column was used.The mobile phase A is 0.1%formic acid(V∶V)aqueous solution,and the mobile phase B is 0.1%formic acid(V∶V)acetonitrile solution.Gradient elution;Column temperature 30℃;Sample size 2μL;Qualitative and quantitative analysis of 3-nitropyrrole and thiourea was performed by ESI source,positive ion mode and multiple reaction monitoring.Results:3-nitropyrrole and thiourea had a good linear relationship with the peak area in the range of 0.03-0.3μg·mL^(-1)(r>0.9995).The average recoveries were 99.06%-100.26%and RSD was 0.02%-0.46%.The limits of detection were 0.0693-0.1407 ng·mL^(-1),and the limits of quantification were 0.2309-0.4690 ng·mL^(-1).UPLC-MS/MS method can be used for rapid qualitative and quantitative screening of 3-nitropyrrole and thiourea.Conclusion:The method is simple,sensitive,convenient,accurate,and the analysis time is as short as 6 min.It can be used for the qualitative and quantitative identification of 3-nitropyrrole and thiourea in pioglitazone hydrochloride tablets.

关 键 词：3-硝基吡咯 硫脲 吡格列酮片 UPLC-MS/MS 定性鉴别 定量检查 

分 类 号：R927.1[医药卫生—药学]