基于超高效液相色谱-飞行时间质谱技术同时定性定量分析复方益肝灵片的化学成分

李颖, 吴茵, 李亚静, 李倩, 王祁民, 董占军

中国医院药学杂志 ›› 2018, Vol. 38 ›› Issue (17) : 1801-1807.

PDF(1080 KB)
PDF(1080 KB)
中国医院药学杂志 ›› 2018, Vol. 38 ›› Issue (17) : 1801-1807. DOI: 10.13286/j.cnki.chinhosppharmacyj.2018.17.07
研究论文

基于超高效液相色谱-飞行时间质谱技术同时定性定量分析复方益肝灵片的化学成分

  • 李颖1, 吴茵2, 李亚静1, 李倩1, 王祁民2, 董占军1,2
作者信息 +

An integrated strategy for qualitative and quantitative profiling of compound Yiganling tablet

  • LI Ying1, WU Yin2, LI Ya-jing1, LI Qian1, WANG Qi-min2, DONG Zhan-jun1,2
Author information +
文章历史 +

摘要

目的:运用超高效液相色谱-飞行时间质谱联用(UPLC-Q-TOF-MS)技术法,对复方益肝灵片中的化学成分进行快速鉴定及定量分析。方法:采用Waters XBridge BEH C18色谱柱(50 mm×2.1 mm,1.7 μm),以0.1%甲酸水-甲醇梯度洗脱,体积流量0.3 mL·min-1;进样量1 μL。质谱采用电喷雾离子源(ESI),正负离子模式下同时采集,通过精确质量数、二级质谱碎片信息和保留时间,参照文献和对照品对化合物进行鉴定;通过Product Ion扫描模式对9种成分进行定量。结果:结合参考文献和对照品信息,共鉴定化合物29个,其中22个化合物来源于五味子,7个化合物来源于水飞蓟素。定量分析方法显示,9种成分在限定质量浓度范围内线性关系良好;加样回收率在96.0%~101.1%,RSD ≤ 3.4%。结论:建立了UPLC-Q-TOF-MS法对复方益肝灵片的成分进行快速分析,为其质量控制及药效机制的阐明提供理论参考。

Abstract

OBJECTIVE To identify and quantify the chemical constituents of compound Yiganling tablets by UPLC-Q-TOF-MS.METHODS Compound Yiganling tablet was analyzed by UPLC-Q-TOF-MS under the both negative and positive ion modes. The chromatographic separation was performed on Waters XBridge BEH C18 column (50 mm×2.1 mm, 1.7 μm) by using a mobile phase consisted of methanol and 0.1% formic acid water at the flow rate of 0.3 mL·min-1 for gradient elution and the injection volume was 1 μL. Quantization was performed by MS/MS using product ion scan mode.RESULTS Twenty-nine compounds were identified. The quantization method performed for analyzing nine compounds in compound Yiganling tablet was systematically validated. The regression equations showing good linear relationships between peak areas and contents of compounds were obtained. The average recoveries of the compounds ranged from 96.0% to 101.1% and the RSD was less than 3.4%.CONCLUSION The developed method is sensitive, accurate and rapid, and can be used for simultaneous qualitative and quantitative analysis of the chemical constituents of compound Yiganling tablets.

关键词

水飞蓟 / 五味子 / 复方益肝灵片 / UPLC-Q-TOF-MS / 化学成分 / 定性 / 定量

Key words

Silybum marianum L. / Schisandra chinensis / compound Yiganling tablet / UPLC-Q-TOF-MS / chemical compounds / qualitative

引用本文

导出引用
李颖, 吴茵, 李亚静, 李倩, 王祁民, 董占军. 基于超高效液相色谱-飞行时间质谱技术同时定性定量分析复方益肝灵片的化学成分[J]. 中国医院药学杂志, 2018, 38(17): 1801-1807 https://doi.org/10.13286/j.cnki.chinhosppharmacyj.2018.17.07
LI Ying, WU Yin, LI Ya-jing, LI Qian, WANG Qi-min, DONG Zhan-jun. An integrated strategy for qualitative and quantitative profiling of compound Yiganling tablet[J]. Chinese Journal of Hospital Pharmacy, 2018, 38(17): 1801-1807 https://doi.org/10.13286/j.cnki.chinhosppharmacyj.2018.17.07
中图分类号: R927.2   

参考文献

[1] Ch.P.Vol Ⅰ(中国药典.一部)[S].2015:67.
[2] Sowndhararajan K, Deepa P, Kim M,et al.An overview of neuroprotective and cognitive enhancement properties of lignans from Schisandra chinensis[J]. Biomed Pharmacother, 2017, 97:958-968.
[3] Xue Y, Li X, Du X,et al.Isolation and anti-hepatitis B virus activity of dibenzocyclooctadiene lignans from the fruits of Schisandra chinensis[J]. Phytochemistry, 2015, 116:253-261.
[4] Chun JN, Cho M, So I,et al.The protective effects of Schisandra chinensis fruit extract and its lignans against cardiovascular disease:a review of the molecular mechanisms.[J]. Fitoterapia, 2014, 97(17):224-233.
[5] Hu D, Yang Z, Yao X,et al. Dibenzocyclooctadiene lignans from Schisandra chinensis and their inhibitory activity on NO production in lipopolysaccharide-activated microglia cells[J]. Phytochemistry, 2014, 104(3):72-78.
[6] Wang XJ. Research on serum pharmacochemistry in Chinese materia medica and Chinese herbal formula[J].World Sci Technol(世界科学技术), 2002,4(2):1-4.
[7] Wang XJ. Methodology for systematic analysis of in vivo efficacy material base of traditional Chinese medicine——Chinmedomics[J]. Chin J Chin Mater Med(中国中药杂志), 2015,(01):13-17.
[8] Shi ZY, Tan J. Determination of schisandrin, schisandrol B and deoxyschizandrin in Fufang Yiganling Pian by HPLC[J]. Cent South Pharm(中南药学), 2011,(4):264-267.
[9] Li W, Song YG, Liu KY,et al. Rapid identification of the different constituents in Fructus Schisandrae Chinensis before and after processing by UHPLC-QTOF/MSE combining with metabonomics[J]. Acta Pharm Sin(药学学报), 2016,(9):1445-1450.
[10] Shi PY, He Q, Zhang YF,et al. Characterisation and identification of isomeric dibenzocyclooctadiene lignans from Schisandra Chinensis by high-performance liquid chromatography combined with electrospray ionisation tandem mass spectrometry.[J].Phytochem Anal, 2009, 20(3):197-206.
[11] Huang X, Song F, Liu Z, et al. Structural characterization and identification of dibenzocyclooctadiene lignans in Fructus Schisandrae using electrospray ionization ion trap multiple-stage tandem mass spectrometry and electrospray ionization Fourier transform ion cyclotron resonance multiple-stage tandem mass spectrometry[J]. Anal Chim Acta, 2008, 615(2):124-135.
[12] Liu K, Song Y, Liu Y, et al. An integrated strategy using UPLC-QTOF-MSE and UPLC-QTOF-MRM (enhanced target) for pharmacokinetics study of wine processed Schisandra Chinensis fructus in rats[J]. J Pharm Biomed Anal, 2017, 139:165-178.
[13] Li Y,Wu Y, Li Q, et al. Identification of chemical constituents in Silymarin Capsules by UPLC-Q-TOF-MS/MS[J]. Chin Hosp Pharm J(中国医院药学杂志), 2017,36(22):2259-2265.

PDF(1080 KB)

130

Accesses

0

Citation

Detail

段落导航
相关文章

/