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.
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)
出处
《药物分析杂志》
CAS
CSCD
北大核心
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]。
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
Gengnianning
Scrophulariae Radix
wine-steamed Ligustri Lucidi Fructus
Codonopsis Radix
Ecliptae Herba
fried Vaccariae Semen
Zingiberis Rhizoma
Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran
harpagide
salidroside
nuezhenide
lobetyolin
wedelolactone
harpagoside
vaccarin
6-gingerol
atractylenolide quality control of Chinese patent medicine
HPLC-MS/MS
作者简介
通信作者:王海波,Tel:(0371)65566577,E-mail:gnn2022gc@163.com;第一作者:蒋芦荻,Tel:(0371)65566040,E-mail:jiangludi_52@163.com。
