小儿咽扁颗粒中掺伪山银花检验方法研究  

Study on the Test Method of Adulterated Lonicerae Flos in Xiaoer Yanbian Granule

作　　者：姜军华 吴良发 许妍 戴忠[2] 周志强 Jiang Junhua;Wu Liangfa;Xu Yan;Dai Zhong;Zhou Zhiqiang(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Chinese Patent Medicine,Jiangxi Province Engineering and Technology Research Center of Drug and Medical Device Quality,Nanchang 330029,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌330029 [2]中国食品药品检定研究院,北京100050

出　　处：《中国药事》2023年第4期443-449,共7页Chinese Pharmaceutical Affairs

基　　金：江西省药品监督管理局科研项目(编号2019JS05)。

摘　　要：目的:建立小儿咽扁颗粒中山银花的高效液相色谱-蒸发光散射检测器(HPLC-ELSD)检查方法,打击中药制剂中金银花的掺假行为。方法:采用薄层色谱(TLC)法,以灰毡毛忍冬皂苷乙为指标成分,以三氯甲烷-甲醇-水(6∶4∶1)为展开剂,快速筛查小儿咽扁颗粒中掺伪的山银花;采用HPLC-ELSD法鉴别小儿咽扁颗粒中掺伪的山银花,选择Sun Fire■C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-水,梯度洗脱,流速1 mL·min^(-1),柱温30℃,进样量10μL;采用高效液相色谱-串联质谱(HPLC-MS)法进行确证,选择Thermo Hypersil GOLD aQ C_(18)(150 mm×2.1 mm,3μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相梯度洗脱,流速0.3 mL·min^(-1),柱温30℃,质谱使用电喷雾离子源,负离子模式下检测。结果:TLC法检测结果显示,34批样品中共有8家企业生产的16批次样品疑似检出灰毡毛忍冬皂苷乙;HPLC-ELSD法的验证结果与TLC法一致,小儿咽扁颗粒中金银花掺伪山银花5%及以上即可检出;16批次检出灰毡毛忍冬皂苷乙样品均得到HPLC-MS法确证。结论:所建系列方法专属性好,灵敏度高,简便、快捷,为打击金银花掺伪提供了有力的技术支撑。Objective:To establish the HPLC-ELSD identification method of Lonicerae Flos in Xiaoer Yanbian granules,crack down on the adulteration of Lonicerae Japonicae Flos in traditional Chinese medicine preparations.Methods:The adulterated Lonicerae Flos in Xiaoer Yanbian granules were quickly screen by TLC with macranthoidin B as the index component and trichloromethane methanol water(6∶4∶1)as the developing agent;The adulterated Lonicerae Flos in Xiaoer Yanbian granules were identified by HPLC-ELSD,a Sun Fire■C_(18)(2)column(4.6 mm×250 mm,5μm)was selected,the mobile phase was acetonitrile-water with gradient elution,the flow rate was 1.0 mL·min^(-1),the column temperature was 30℃,and the sample volume was 10μL;it was confirmed by LC-MS,and the column was Thermo Hypersil GOLD aQ C_(18)(150 mm×2.1 mm,3μm)gradiently eluted with acetonitrile-0.1%formic acid solution as the mobile phase at the flow rate of 0.3 mL·min^(-1),and the column temperature was 30℃.Electrospray ion source was used for mass spectrometer,detected in negative ion mode.Results:TLC test results showed that a total of 16 batches of 34 samples produced by 8 enterprises were suspected of detecting macranthoidin B;the verification result of HPLC-ELSD method were consistent with TLC method,and 5% or more of Lonicerae Flos mixed with Lonicerae Japonicae Flos in Xiaoer Yanbian granules could be detected.The 16 batches of macranthoidin B samples were confirmed by HPLC-MS.Conclusion:The established series of methods have good specificity,high sensitivity,simplicity and rapidity,and it provides a strong technical support for combating Lonicerae Japonicae Flos adulteration.

关 键 词：小儿咽扁颗粒 金银花 山银花 灰毡毛忍冬皂苷乙 高效液相色谱-蒸发光散射检测器法 

分 类 号：R917[医药卫生—药物分析学]