消风止痒颗粒中水防风掺伪检测方法研究  

Research on detection method of adulteration of Libanotis laticalycina in Xiaofeng Zhiyang Granules

作　　者：蔡艳丽 李翠华 李正国 CAI Yanli;LI Cuihua;LI Zhengguo(Jining Institute for Food and Drug Control,Shandong,Jining 272000,China)

机构地区：[1]山东省济宁市食品药品检验检测研究院,山东济宁272000

出　　处：《中国医药科学》2024年第19期47-50,共4页China Medicine And Pharmacy

基　　金：2023年山东省药品质量风险监测项目。

摘　　要：目的建立消风止痒颗粒中水防风高效液相色谱(HPLC)检测方法。方法以水防风特征性成分3’(R),4’(R)-双当归酰氧基-3’,4’-二氢花椒内酯为指标,采用HPLC进行测定。色谱柱为Hypersil Gold AQ C18(250 mm×4.6 mm,5μm),以乙腈-水为流动相进行梯度洗脱,检测波长为324 nm。通过保留时间和紫外吸收光谱进行定性,峰面积外标法进行定量。检测的阳性样品以高效液相色谱-串联质谱(HPLC-MS/MS)进行确证。采用电喷雾离子源,正离子模式,选择反应监测模式扫描方法。结果水防风特征性成分能完全分离,在0.53~26.55μg/ml范围内线性关系良好,回收率平均值为96.06%,RSD为2.0%;检出限为1.0 ng,定量限为3.3 ng。50批次消风止痒颗粒中检出1批次阳性样品,超过拟定限度,存在掺伪情况。结论该方法灵敏度高、实用性强,可作为消风止痒颗粒中防风的补充检验方法。Objective To establish a high-performance liquid chromatography(HPLC)method for the determination of Libanotis laticalycina in Xiaofeng Zhiyang Granules.Methods The characteristic components of 3’(R),4’(R)-bis-angelica acyloxy-3’,4’-dihydroZanthoxylactone of Libanotis laticalycina were determined by HPLC.The chromatographic column was Hypersil Gold AQ C18(250 mm×4.6 mm,5μm),the gradient elution was carried out with acetonitrile-water as mobile phase,and the detection wavelength was 324 nm.Qualitative analysis was carried out by retention time and ultraviolet absorption spectrum,and quantitative analysis was carried out by peak area external standard method.Positive samples were confirmed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Using electrospray ion source and positive ion mode,reaction monitoring mode scanning method was selected.Results The characteristic components of Libanotis laticalycina can be completely separated,and the linear relationship was good in the range of 0.53-26.55μg/ml.The average recovery rate was 96.06%and RSD was 2.0%.The detection limit was 1.0 ng and the quantitative limit was 3.3 ng.1 batch of positive samples was detected in 50 batches of Xiaofeng Zhiyang Granules,which exceeded the proposed limit and was adulterated.Conclusion This method is sensitive and practical,and can be used as a supplementary test method for Libanotis laticalycina in Xiaofeng Zhiyang Granules.

关 键 词：消风止痒颗粒 水防风 3’(R) 4’(R)-双当归酰氧基-3’ 4’-二氢花椒内酯 高效液相色谱 高效液相色谱-串联质谱 

分 类 号：R284.1[医药卫生—中药学]