HPLC-MS/MS法同时测定更年宁中11个成分  

Simultaneous determination of 11 components in Gengnianning by HPLC-MS/MS

作　　者：蒋芦荻 王晓燕 刘亚楠 王海波 杨琰 李海燕 JIANG Lu-di;WANG Xiao-yan;LIU Ya-nan;WANG Hai-bo;YANG Yan;LI Hai-yan(Henan Institute for Drug and Medical Device Inspection,State Drug Administration Key Laboratory of Quality Control of Chinese Herbal Medicines and Decoction Pieces,Zhengzhou 450018,China)

机构地区：[1]河南省药品医疗器械检验院国家药品监督管理局中药材及饮片质量控制重点实验室,郑州450018

出　　处：《药物分析杂志》2024年第5期827-834,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：2022年国家药品抽检(中央补助地方经费项目)(No.41);河南省市场监督管理局科技计划项目(2023sj61);中国药品监管科学行动计划第二批重点项目[NMPAJGKX-2023-028]。

摘　　要：目的:建立HPLC-MS/MS法同时测定更年宁中哈巴苷、红景天苷、特女贞苷、党参炔苷、蟛蜞菊内酯、哈巴俄苷、王不留行黄酮苷、6-姜辣素、白术内酯Ⅲ、白术内酯Ⅱ、白术内酯Ⅰ共11个成分的含量。方法:采用C18色谱柱(100 mm×2.1 mm,1.9μm),以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,流速为0.3 mL·min^(-1),柱温为25℃,进样量为1μL;质谱采用电喷雾离子源(ESI),电离模式为ESI-(哈巴苷、红景天苷、特女贞苷、党参炔苷、蟛蜞菊内酯、哈巴俄苷)和ESI+(王不留行黄酮苷、6-姜辣素、白术内酯Ⅲ、白术内酯Ⅱ、白术内酯Ⅰ),多反应监测(MRM)模式进行定量分析。结果:11个成分的线性范围分别为1.485~29.71、1.620~32.40、7.801~156.0、0.518~10.35、0.167~3.333、0.359~7.179、1.455~29.10、1.520~30.40、0.160~3.205、0.143~2.864、0.157~3.136μg·mL^(-1),r均≥0.9980;平均回收率(n=6)在95.9%~102.6%,RSD在0.90%~3.0%。5个企业生产的10批更年宁样品中上述11个成分的含量分别为14.8~104.5、37.6~288.5、335.8~1332.8、6.2~10.1、6.6~61.8、13.7~75.1、57.4~132.8、16.9~70.6、11.8~33.9、3.4~15.4、6.5~12.9μg·g^(-1)。结论:本方法灵敏、准确,可用于更年宁的质量控制。Objective:To establish an HPLC-MS/MS method for simultaneous determination of 11 components(harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atractylenolideⅢ,atractylenolideⅡ,and atractylenolideⅠ)in Gengnianning.Methods:HPLC assay was performed on C_(18)column(100 mm×2.1 mm,1.9μm)with a mixture of methanol and 0.1%formic acid as the mobile phase in gradient elution at a flow rate of 0.3 mL·min^(-1).The column temperature was 25℃and the injection volume was 1μL.Detection was carried out on a triple quadrupole mass spectrometer in positive ion mode(harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone and harpagoside)and negative ion mode(vaccarin,6-gingerol,atractylenolideⅢ,atractylenolideⅡ,and atractylenolideⅠ)using an electrospray ion source(ESI).Multiple reaction monitoring(MRM)mode was employed.Results:The calibration curves were linear within the ranges of 1.485-29.71μg·mL^(-1),1.620-32.40μg·mL^(-1),7.801-156.0μg·mL^(-1),0.518-10.35μg·mL^(-1),0.167-3.333μg·mL^(-1),0.359-7.179μg·mL^(-1),1.455-29.10μg·mL^(-1),1.520-30.40μg·mL^(-1),0.160-3.205μg·mL^(-1),0.143-2.864μg·mL^(-1)and 0.157-3.136μg·mL^(-1)for harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atractylenolideⅢ,atractylenolideⅡ,and atractylenolideⅠ,respectively.All 11 components showed good linearity(r≥0.9980).The average recoveries(n=6)were in the range of 95.9%-102.6%with RSDs within 0.90%-3.0%.The contents of harpagide,salidroside,nuezhenide,lobetyolin,wedelolactone,harpagoside,vaccarin,6-gingerol,atractylenolideⅢ,atractylenolideⅡand atractylenolideⅠin 10 tested samples from 5 manufactures were 14.8-104.5,37.6-288.5,335.8-1332.8,6.2-10.1,6.6-61.8,13.7-75.1,57.4-132.8,16.9-70.6,11.8-33.9,3.4-15.4 and 6.5-12.9μg·g^(-1).Conclusion:The developed method is accurate and sensitive.It can be used in quality control of Gengnianning.

关 键 词：更年宁 玄参 酒女贞子 党参 墨旱莲 炒王不留行 干姜 麸炒白术 哈巴苷 红景天苷 特女贞苷 党参炔苷 蟛蜞菊内酯 哈巴俄苷 王不留行黄酮苷 6-姜辣素 白术内酯 中成药质量控制 高效液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]