首页|酸枣仁与理枣仁鉴别方法研究

酸枣仁与理枣仁鉴别方法研究

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  • 国家科技期刊平台
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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.
Identification Methods of Ziziphi Spinosae Semen and Ziziphi Mauritianae Semen
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.

Ziziphi Spinosae SemenZiziphi Mauritianae SemenUPLC-MS/MSmorphological identificationmicroscopic identification6'''-sinapoylspinosin

张艳慧、张明童、刘丽丽、王楠

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河北省保定市食品药品检验所,河北 保定 071000

甘肃省药品检验研究院·甘肃省中藏药检验检测技术工程实验室·国家药品监督管理局中药材及饮片质量控制重点实验室,甘肃 兰州 730070

河北省石家庄海关技术中心保定业务部,河北 保定 071051

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

河北省市场监督管理局科研项目甘肃省药品监督管理局药品科研项目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甘肃省兰州市科技计划

2020ZD362022GSMPA00172022GSMPA-KL122022GSMPA-KL102022-3-41

2024

10.3969/j.issn.1006-4931.2024.01.015

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子：1.369
ISSN：1006-4931
年,卷(期)：2024.33(1)
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