龙泽熊胆胶囊中水防风掺伪的检测方法研究  

Determination of Libanotis laticalycina Adulterated in Longze Xiongdan Capsules

作　　者：刘珍[1] 陆佳 张万青 苏章轩 吴群悦 刘潇潇[1] LIU Zheng;LU Jia;ZHANG Wanqing;SU Zhangxuan;WU Qunyue;LIU Xiaoxiao(Guangdong Drug Inspection Institute,Guangzhou 510663 Guangdong,China)

机构地区：[1]广东省药品检验所,广东广州510663

出　　处：《中药新药与临床药理》2024年第4期570-579,共10页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：广东省药品监督管理局科技创新项目(2023YDZ03);广东省医学科研基金项目(B2023258)。

摘　　要：目的建立龙泽熊胆胶囊中水防风掺伪的检测方法。方法以水防风区别于防风的专属性成分Xanthalin建立薄层色谱鉴别法(TLC),对样品进行初筛。若供试品溶液色谱中出现水防风特征斑点,则采用高效液相色谱(HPLC)进行定性检查。色谱条件:SHIMADZU InertSustain~?C18色谱柱(250 mm×4.6 mm,5μm);以乙腈-水(58∶42)为流动相,等度洗脱;流速:1.0 mL·min^(-1);柱温:30℃;检测波长:324 nm;进样量:10μL。若供试品Xanthalin色谱峰面积大于对照品的峰面积,视为阳性检出,必要时可进一步采用超高效液相色谱串联三重四级杆质谱法(UPLC-MS/MS)进一步确证。结果建立的TLC法、HPLC法简便、快速,专属性、重复性、耐用性均符合《中国药典》要求。对市售107批龙泽熊胆胶囊样品进行检测,19批次样品检出Xanthalin,提示该制剂存在水防风掺伪投料生产的风险。结论该方法可实现水防风掺伪防风的定性鉴别,有助于完善该品种的质量控制。To establish analytical methods of Libanotis laticalycina adulterated in Longze Xiongdan Capsules.Methods Utilizing the characteristic component of Libanotis laticalycina(Xanthalin)to develop TLC method,the initial screening of the sample was performed.If the characteristic spot of Xanthalin was found,the analysis was carried out by HPLC.HPLC method was performed on SHIMADZU InertSustain®C18(250 mm×4.6 mm,5μm)column with acetonitrile-water(58∶42)as mobile phase by isocratic elution at a flow rate of 1.0 mL·min^(-1).The column temperature was 30℃,the detection wavelength was set at 324 nm,and the sample injection volume was 10μL.When the chromatographic peak area of Xanthalin in test samples was greater than that in reference samples,it suggested that Libanotis laticalycina was used to adulterate in Longze Xiongdan Capsules.If necessary,ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)could be used for further confirmation.Results TLC and HPLC methods are simple and fast.The specificity,repeatability and durability all met the requirements of“Chinese Pharmacopoeia”.The result showed that Xanthalin in 19 batches of samples was detected in 107 batches of Longze Xiongdan Capsules,which indicated that there was a risk of the adulteration of Libanotis laticalycina in production of Longze Xiongdan Capsules.Conclusion The method could be applied to inspect Libanotis laticalycina adulterated in Longze Xiongdan Capsules qualitatively,which could improve the quality control of this preparation.

关 键 词：龙泽熊胆胶囊 防风 水防风 掺伪 Xanthalin 

分 类 号：R284.1[医药卫生—中药学]