中国药业2024，Vol.33Issue(1)：68-72,5.DOI:10.3969/j.issn.1006-4931.2024.01.015
酸枣仁与理枣仁鉴别方法研究
Identification Methods of Ziziphi Spinosae Semen and Ziziphi Mauritianae Semen
摘要
Abstract
Objective To establish a method for the identification of Ziziphi Spinosae Semen(ZSS)and Ziziphi Mauritianae Semen(ZMS),and to provide a basis for quality control and market supervision of ZSS.Methods Morphological and microscopic identification of ZSS and ZMS was conducted.The content of 6'''-sinapine in ZSS and ZMS was determined by the ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method,the chromatographic column was Phenonex C18 column(100 mm×2.1 mm,2.6 μm),the mobile phase was 0.1%formic acid-10 mmol/L ammonium formate aqueous solution-methanol(gradient elution),the flow rate was 0.2 mL/min,the column temperature was 30℃,the injection volume was 5 μL,multi-reaction monitoring mode scanning adopted with electric spray ion source and positive ion,the electric spray voltage was 3.5 kV,the ion source temperature was 150℃,the desolvent gas temperature was 500℃,and the scanning range was 50-1 000 amu.Results There were differences in the texture of the exotesta between ZSS and ZMS in terms of traits,as well as differences in the grid like cells of the exotesta and the inner epidermal cells of the testa in terms of microscopic characteristics.The linear range of 6'''-sinapoylspinosin was 0.205 2-6.156 μg/mL(r = 0.997 5,n = 6).The limit of detection(LOD)was 21.13 pg.The RSDs of precision,stability,and repeatability test results of ZSS and ZMS samples were lower than 3.0%(n = 6).The recovery rates of 6'''-sinapoylspinosin in ZSS and AMS were 97.01%and 97.80%with RSDsof 2.15%and 2.09%(n = 6),respectively.The content of 6'''-sinapoylspinosin in ZSS and ZMS in 10 batches of samples were 0.23 μg/mL and 3.70 μg/mL,respectively.The limit of ZMS in ZSS was set as 5%.When the content of 6'''-sinapoylspinosin in the sample was higher than 0.5 μg/mL,which could be considered adulterating ZMS.Conclusion The established method is simple and accurate with good repeatability and stability,which can effectively distinguish ZSS and ZMS.关键词
酸枣仁/理枣仁/超高效液相色谱串联质谱法/性状鉴别/显微鉴别/6'''-芥子酰斯皮诺素Key words
Ziziphi Spinosae Semen/Ziziphi Mauritianae Semen/UPLC-MS/MS/morphological identification/microscopic identification/6'''-sinapoylspinosin分类
医药卫生引用本文复制引用
张艳慧,张明童,刘丽丽,王楠..酸枣仁与理枣仁鉴别方法研究[J].中国药业,2024,33(1):68-72,5.基金项目
河北省市场监督管理局科研计划项目[2020ZD36] （）
甘肃省药品监督管理局药品科研项目[2022GSMPA0017] （）
甘肃省药品监督管理局中药材及饮片质量控制重点实验室项目[2022GSMPA-KL12,2022GSMPA-KL10] （）
甘肃省兰州市科技计划项目[2022-3-41]. （）
