溴芬酸钠滴眼液中2-吡咯烷酮的定性定量方法研究  

Investigation on qualitative and quantitative methods of 2-pyrrolidone in brofenac sodium eye drops

作　　者：吴永芹 王雪云 杨芳 徐魁 崔效廷 WU Yongqin;WANG Xueyun;YANG Fang;XU Kui;CUI Xiaoting(Jining Food and Drug Inspection and Testing Research Institute,Jining 272073,China;Cisen Pharmaceutical Co.,Ltd,Jining 272073,China)

机构地区：[1]济宁市食品药品检验检测研究院,山东济宁272073 [2]辰欣药业股份有限公司,山东济宁272073

出　　处：《中国药品标准》2023年第5期520-524,共5页Drug Standards of China

基　　金：2020年山东省药品质量风险监测项目(No.21)。

摘　　要：目的:建立溴芬酸钠滴眼液中2-吡咯烷酮的HPLC含量测定方法和LC-MS/MS定性方法。方法:采用色谱柱Waters XTERRAC_(18)(4.6 mm×250 mm,5μm),柱温30℃,流动相A 0.05 mol·L^(-1)磷酸氢二钾溶液(pH 6.0)-乙腈(95∶5),流动相B 0.05 mol·L^(-1)磷酸氢二钾溶液(pH 6.0)-乙腈(30∶70)梯度洗脱,流速1.0 mL·min^(-1),检测波长205 nm。LC-MS/MS方法采用梯度洗脱,全扫描和选择离子监测,正离子模式,对2-吡咯烷酮进行定性分析。结果:2-吡咯烷酮在1.08~216.0μg·mL^(-1)(r=0.9994)范围内线性关系良好,平均加样回收率(n=9)为102.7%,RSD为2.3%。LC-MS/MS法可以对2-吡咯烷酮进行快速定性鉴别。结论:建立的定性与定量方法准确、简便、快速,可用于溴芬酸钠滴眼液中2-吡咯烷酮的含量测定和定性鉴别。Objective:To establish an HPLC content determination method and an LC-MS/MS qualitative method for the determination of 2-pyrrolidone in brofenac sodium eye drops.Methods:The chromatography was performed on Waters XTERRAC_(18)(4.6 mm×250 mm,5μm)column at 30℃.Mobile phase A 0.05 mol·L^(-1)dipotassium phosphate solution(pH 6.0)-acetonitrile(95∶5),mobile phase B 0.05 mol·L^(-1)dipotassium phosphate solution(pH 6.0)-acetonitrile(30∶70)gradient elution,flow rate 1.0 mL·min^(-1),detection wavelength 205 nm.The LC-MS/MS method was used for qualitative analysis of 2-pyrrolidone by gradient elution,full scanning and selective ion monitoring,and positive ion mode.Results:2-Pyrrolidone had a good linear relationship in the range of 1.08-216.0μg·mL^(-1)(r=0.9994),and the average dosing recovery rate(n=9)was 102.7%and RSD was 2.3%.The LC-MS/MS method enables rapid qualitative identification of 2-pyrrolidone.Conclusion:The established qualitative and quantitative methods are accurate,simple and rapid,and can be used for the determination and qualitative identification of 2-pyrrolidone in brofenac sodium eye drops.

关 键 词：2-吡咯烷酮 溴芬酸钠滴眼液 HPLC LC-MS/MS 含量测定 定性鉴别 

分 类 号：R921.2[医药卫生—药学]