食品科学 ›› 2013, Vol. 34 ›› Issue (22): 150-153.doi: 10.7506/spkx1002-6630-201322030

• 分析检测 • 上一篇    下一篇

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

马桂劼,张 婷,解军波,庞广昌   

  1. 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
  • 收稿日期:2013-06-17 修回日期:2013-10-16 出版日期:2013-11-25 发布日期:2013-12-05
  • 通讯作者: 解军波 E-mail:xjbo@tjcu.edu.cn
  • 基金资助:

    国家自然科学基金青年科学基金项目

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

MA Gui-jie,ZHANG Ting,XIE Jun-bo,PANG Guang-chang   

  1. 1. School of Biotechnology and Food Science, Tianjin University of Commerce, Tianjin 300134, China;
    2. Tianjin Key Laboratory of Food Biotechnology, Tianjin 300134, China
  • Received:2013-06-17 Revised:2013-10-16 Online:2013-11-25 Published:2013-12-05

摘要:

目的:建立高效液相色谱-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YMC ODS-AQTM 色谱柱,乙腈-0.1%甲酸溶液(36:64,V/V)为流动相,流速0.3mL/min,柱温30℃,进样量20μL;ESI负离子模式下,采用多重反应监测模式,监测的离子为m/z 1205.6~1073.6(皂苷A),m/z 1043.6~911.7(皂苷B),m/z 607.2~427.0(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(r>0.9992),平均加样回收率分别为97.39%、97.86%和98.48%,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21.46mg/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。

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

Abstract:

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 ODSAQ
TM column with acetonitrile-0.1% formic acid (36:64, V/V) 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.

Key words: Ziziphi Spinosae Semen (ZSS) dispersible tablet, jujuboside A (JuA), jujuboside B (JuB), spinosin, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS), multiple reaction monitoring (MRM)

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