HPLC-MS/MS测定酸枣仁和理枣仁中<i>O</i>-去甲荷叶碱

依泽; 周颖; 王荣; 陆静娴; 焦阳; 郑成; 陈碧莲

doi:10.13748/j.cnki.issn1007-7693.20241228

HPLC-MS/MS测定酸枣仁和理枣仁中O-去甲荷叶碱

Determination of O-Nornuciferine in Ziziphi Spinosae Semen and Ziziphi Mauritianae Semen by HPLC-MS/MS

摘要

摘要:
目的建立HPLC-MS/MS测定酸枣仁及理枣仁中O-去甲荷叶碱含量的方法。
方法采用Phenomenex Kinetex C₁₈色谱柱(100 mm×2.1 mm，2.6 μm)；流动相为甲醇-乙腈-0.1%甲酸水溶液(7.5∶7.5∶85)，流速为0.3 mL·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。
结果 O-去甲荷叶碱的进样量在0.00049~0.98 ng(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。

Abstract:
OBJECTIVE To establish an HPLC-MS/MS method for the determination of O-Nornuciferine in Ziziphi Spinosae Semen and Ziziphi mauritianae Semen.
METHODS Phenomenex Kinetex C₁₈ column(100 mm×2.1 mm, 2.6 μm) 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 0.3 mL·min⁻¹. Electrospray positive ion(ESI⁺) source was used for mass spectrometry detection by multiple reaction monitoring mode.
RESULTS The liner range of calibration curve was 0.00049–0.98 ng(r=0.9992). The RSD of repeatability test was 4.2%. The average recovery was 87.0%, RSD was 1.5%. The limit of detection and quantitation were 0.116 ng·g⁻¹ and 0.386 ng·g⁻¹.
CONCLUSION The method has well specificity, sensitivity and applicable, which provides reference for quality control of Ziziphi Spinosae Semen.

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