HPLC-MS-MS法同时测定酸枣仁分散片中酸枣仁皂苷A、酸枣仁皂苷B、斯皮诺素的含量  

Simultaneous Determination of Jujuboside A,Jujuboside B and Spinosin in Ziziphi Spinosae Semen Dispersible Tablets by HPLC-MS-MS

作　　者：马桂劼 张婷[1] 解军波[1,2] 庞广昌[1,2] 

机构地区：[1]天津商业大学生物技术与食品科学学院,天津300134 [2]天津市食品生物技术重点实验室,天津300134

出　　处：《食品科学》2013年第22期150-153,共4页Food Science

基　　金：国家自然科学基金青年科学基金项目(31000749)

摘　　要：目的：建立高效液相色谱一电喷雾电离质谱法同时测定酸枣仁分散片中酸枣仁皂苷A、酸枣仁皂苷B、斯皮诺素含量的方法。方法：采用YMCODS．AQ^TM色谱柱，乙腈．0．1％甲酸溶液（36：64，V／功为流动相，流速0．3mL／min，柱温30℃，进样量20止；ESI负离子模式下，采用多重反应监测模式，监测的离子为m／z1205．6～1073．6（皂苷A），m／z1043．6～911．7（皂苷B），m／z607．2-427．0（斯皮诺素）。结果：分散片中酸枣仁皂苷A、酸枣仁皂苷B和斯皮诺素含量与峰面积的线性关系良好驴〉0．9992），平均加样回收率分别为97．39％、97．86％3198．48％，相对标准偏差均小于1．0％。酸枣仁分散片中3种组分的含量分别为4．15、1．46mg／g和2 1．46mg／g。该方法快捷、准确、重复性好，可用于酸枣仁分散片中酸枣仁皂苷A、酸枣仁皂苷B和斯皮诺素的同时测定。Abstraet： Objective： A method for simultaneous determination of jujuboside A （JuA）, jujuboside B （JuB） and spinosin in ZSS （Ziziphi Spinosae Semen） dispersible tablets was established using high performance liquid chromatography tandem electrospray ionization mass spectrometry （HPLC-ESI-MS-MS）. Methods： The separation was performed on a YMC ODS- AQTM column with acetonitrile-0.1% formic acid （36：64, V/F） as the mobile phase at flow rate of 0.3 mL/min. The column temperature was 30 ℃. The injection volume was 20 μL. The analytes were detected by ESI-MS in the negative ion mode. In the multiple reaction monitoring （MRM） mode, the quantitative determination of JuA at m/z of 1205.6-1073.6, JuB at m/z of 1043.6-911.7, spinosin at m/z of 607.2-427.0 was carried out. Results： A good linear relationship between the peak area and the concentrations of JuA, JuB and spinosin was obtained （r 〉 0.9992）. The average recovery rates for them were 97.39%, 97.86% and 98.48%, respectively, with relative standard deviation less than 1.0%. The contents of JuA, JuB and spinosin in ZSS dispersible tablets were 4.15, 1.46 mg/g and 21.46 mg/g, respectively. The developed method is rapid, accurate and repeatable, which is suitable for the simultaneous determination of JuA, JuB and spinosin in ZSS dispersible tablets.

关 键 词：酸枣仁分散片 酸枣仁皂苷A 酸枣仁皂苷B 斯皮诺素 液相色谱串联质谱法 多重反应监测 

分 类 号：R944.4[医药卫生—药剂学]