中国中药杂志

2011, v.36(06) 702-705

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UPLC-MS同时测定千里光和欧洲千里光中阿多尼弗林碱和千里光碱的含量
Simultaneous quantitation of adonifoline and senecionine in Senecio herbs by UPLC-MS

熊爱珍;杨莉;杨雪晶;王长虹;王峥涛;
XIONG Aizhen1,YANG Li1*,YANG Xuejing2,WANG Changhong1,WANG Zhengtao1,2,3(1.MOE Key Laboratory for Standardization of Chinese Medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;2.Department of Pharmacognosy,China Pharmaceutical University, Nanjing 210038,China;3.Shanghai Key Laboratory for Compound Chinese medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China)

摘要(Abstract):

目的:建立同时测定千里光和欧洲千里光中阿多尼弗林碱和千里光碱含量的UPLC-MS方法。方法:采用Wa-ters公司UPLC-Micro 2000仪器ESI+离子模式下选择离子监控,以野百合碱为内标计算浓度;色谱分离采用Shiseido CapcellPak MG色谱柱(2.0 mm×50 mm,3μm),流动相乙腈-0.5%甲酸水溶液梯度洗脱,流速0.3 mL.min-1,柱温30℃,进样量2μL。结果:阿多尼弗林碱进样质量浓度在1.02~816.00μg.L-1呈现良好线性关系(r=0.998 0),50%,100%,150%浓度水平下加样回收率在95.73%~103.0%,RSD不超过2.5%;千里光碱进样质量浓度在1.08~860.56μg.L-1呈现良好线性关系(r=0.997 6),50%,100%,150%浓度水平下加样回收率在95.67%~101.5%,RSD不超过2.3%;方法重复性及精密度良好。结论:所建立UPLC-MS方法灵敏、准确,重现性好,适用于千里光和欧洲千里光中阿多尼弗林碱和千里光碱的含量测定,可用于千里光药材中吡咯里西啶类生物碱的限量检查以及其混用品种如欧洲千里光的监控,为千里光药材2010年版《中国药典》的质量标准研究奠定基础。
Objective: To develop an UPLC-MS method for the simultaneously quantitation of adonifoline and senecinine in Senecio herbs.Method: UPLC-Micro 2000 was used for quantification in SIR mode under ESI+.Monocrotaline was used as the internal standard.Chromatography was performed on a Shiseido Capcell Pak MG(2.0 mm×50 mm,3 μm) column at 30 ℃ using an gradient elution of acetonitrile-0.5% formic acid in water at the flow rate of 0.3 mL·min-1.The injection volume was 2 μL.Result: Good linearity was obtained for quantitation of adonifoline over the range of 1.02-816.00 μg·L-1(r=0.998 0).And recoveries at different concentration levels were between 95.73% and 103.0% with RSDs no more than 2.5%.For quantification of senecionine,the linear range was between 1.08-860.56 μg·L-1(r=0.997 6).And recoveries at different concentration levels were between 95.67% and 101.5% with RSDs no more than 2.3%.Good reproducibility and precision were also achieved.Conclusion: The new developed UPLC method is sensitive,accurate and reliable enough for the quantitation of adonifoline and senecionine in Senecio herbs thus can be used for the limit detection of pyrrolizidne alkaloids in S.scandens.It can also be used for the identification of fake drugs of S.scandens such as S.vulgaris.The developed method was served for the quality evaluation of Herba Senecionis Scandentis.

关键词(KeyWords): 千里光;欧洲千里光;吡咯里西啶类生物碱;液质联用
Senecio scandens;Senecio vulgaris;pyrrolizidine alkaloids;UPLC-MS

Abstract:

Keywords:

基金项目(Foundation): 国家“重大新药创制”科技重大专项(2009ZX09308-003,2009ZX09052-013,2009ZX09052-021,2009ZX09052-024);; 国家自然科学基金项目(30701104);; 上海市国际合作基金项目(09540704700)

作者(Author): 熊爱珍;杨莉;杨雪晶;王长虹;王峥涛;
XIONG Aizhen1,YANG Li1*,YANG Xuejing2,WANG Changhong1,WANG Zhengtao1,2,3(1.MOE Key Laboratory for Standardization of Chinese Medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;2.Department of Pharmacognosy,China Pharmaceutical University, Nanjing 210038,China;3.Shanghai Key Laboratory for Compound Chinese medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China)

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