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引用本文:依泽,周颖,王荣,陆静娴,焦阳,郑成,陈碧莲.HPLC-MS/MS法测定酸枣仁和理枣仁中O-去甲荷叶碱[J].中国现代应用药学,2025,42(17):156-155.
YI ZE,ZHOU YING,WANG RONG,LU JINGXIAN,JIAO YANG,ZHENG CHENG,CHEN BILIAN.Determination of O-Nornuciferine in Ziziphi Spinosae Semen and Ziziphi mauritianae Semen by HPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2025,42(17):156-155.
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HPLC-MS/MS法测定酸枣仁和理枣仁中O-去甲荷叶碱
依泽1, 周颖1, 王荣1, 陆静娴1, 焦阳2, 郑成1, 陈碧莲1
1.浙江省食品药品检验研究院;2.山东省食品药品检验研究院
摘要:
目的 建立HPLC-MS/MS法测定酸枣仁及理枣仁中O-去甲荷叶碱的含量。方法 采用C18色谱柱(内径2.1mm);流动相为甲醇-乙腈-0.1%甲酸水溶液(7.5: 7.5: 85),流速为0.3mL·min-1;采用质谱检测器,电喷雾正离子(ESI+)模式,进行多反应监测(MRM)。结果 O-去甲荷叶碱的进样量在0.00049ng~0.98ng(r=0.9992)内有良好的线性关系。重复性试验RSD为4.2%,平均回收率为87.0%,RSD为1.5%,检测限为0.116 ng·g-1,定量限为0.386 ng·g-1。结论 该方法专属性好,灵敏度高,适用性强,可为酸枣仁的质量控制提供参考。
关键词:  酸枣仁  理枣仁  O-去甲荷叶碱  掺伪  HPLC-MS/MS
DOI:
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基金项目:
Determination of O-Nornuciferine in Ziziphi Spinosae Semen and Ziziphi mauritianae Semen by HPLC-MS/MS
YI ZE1, ZHOU YING1, WANG RONG1, LU JINGXIAN1, JIAO YANG2, ZHENG CHENG1, CHEN BILIAN1
1.Zhejiang Institute for Food and Drug Control;2.Shandong Institute for Food and Drug Control
Abstract:
OBJECTIVE To establish an HPLC-MS/MS method for the determination of O-Nornuciferine in Ziziphi Spinosae Semen and Ziziphi mauritianae Semen. METHOD C18 column (inner diameter was 2.1mm) was used for separation. The mobile phase consist of methnol, acetonitrile and 0.1% formic acid-H2O (7.5: 7.5: 85). The flow rate was 0.3mL·min-1. Electrospray positive ion source was used for mass spectrometry detection by multiple reaction monitoring mode. RESULTS The liner range of calibration curve was 0.00049ng~0.98ng (R=0.9992). The RSD of repeatability test was 4.2%. The average recoveries was 87.0%, RSD was 1.5%. The limit of detection and quantitation were 0.116ng·g-1 and 0.386 ng·g-1. CONCLUSION The method has well specificity, sensitivity and applicable, which provided reference for quality control of Ziziphi Spinosae Semen.
Key words:  Ziziphi Spinosae Semen  Ziziphi mauritianae Semen  O-Nornuciferine  adulteration  HPLC-MS/MS
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