摘要
目的 建立酸枣仁及常见伪品理枣仁的鉴别方法,为酸枣仁的质量控制和市场监督提供依据。方法 对酸枣仁和理枣仁进行性状及显微鉴别,采用超高效液相色谱串联质谱(UPLC-MS/MS)法测定其中6’’’-芥子酰斯皮诺素的含量,色谱柱为Phenomenex C18柱(100 mm×2.1 mm,2.6μm),流动相为0.1%甲酸-10 mmol/L甲酸铵水溶液-甲醇(梯度洗脱),流速为0.2 mL/min,柱温为30℃,进样量为5μL,离子源为电喷雾离子源,正离子、多反应监测模式扫描,电喷雾电压为3.5 kV,离子源温度为150℃,去溶剂气温度为500℃,扫描范围为50~1 000 amu。结果 酸枣仁和理枣仁在性状上外种皮纹理存在差异,在显微特征上外种皮栅状细胞、种皮内表皮细胞存在差异。6’’’-芥子酰斯皮诺素的质量浓度在0.205 2~6.156μg/mL范围内与峰面积积分值线性关系良好(r=0.997 5,n=6),检测限为21.13 pg。酸枣仁和理枣仁样品的精密度、稳定性、重复性试验结果的RSD均低于3.0%(n=6);加样回收率分别为97.01%和97.80%,RSD分别为2.15%和2.09%(n=6)。10批酸枣仁和理枣仁中6’’’-芥子酰斯皮诺素的含量分别为0.23,3.70μg/mL。拟订酸枣仁中掺伪理枣仁限度为5%,样品中6’’’-芥子酰斯皮诺素测得含量大于0.5μg/mL时可视为掺伪理枣仁。结论 所建立的方法操作简便、结果准确、重复性和稳定性均良好,可有效鉴别酸枣仁和理枣仁。
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 C_(18) column(100 mm×2.1 mm,2.6μm),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 5μL,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 50-1000 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 0.2052-6.156μg/mL(r=0.9975,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 RSDs of 2.15%and 2.09%(n=6),respectively.The content of 6'''-sinapoylspinosin in ZSS and ZMS in 10 batches of samples were 0.23μg/mL and 3.70μg/mL,respectively.The limit of ZMS in ZSS was set as 5%.When the content of 6'''-sinapoylspinosin in the sample was higher than 0.5μg/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.
作者
张艳慧
张明童
刘丽丽
王楠
ZHANG Yanhui;ZHANG Mingtong;LIU Lili;WANG Nan(Baoding Institute for Food and Drug Control,Baoding,Hebei,China 071000;Gansu Institute for Drug Control·Gansu Inspection and Testing Technical Engineering Laboratory for Chinese Herbal and Tibetan Medicine·NMPA Key Laboratory for Quality Control of TCM,Lanzhou,Gansu,China 730070;Baoding Business Department of Shijiazhuang Customs Technology Center,Baoding,Hebei,China 071051)
出处
《中国药业》
CAS
2024年第1期68-72,共5页
China Pharmaceuticals
基金
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]。
