目的 建立同时测定小金丸中7种成分(麝香酮、次乌头碱、乌头碱、原儿茶酸、阿魏酸、藁本内酯和11-羰基-β-乙酰乳香酸) 含量的超高压液相色谱串联四级杆飞行时间质谱联用( UPLC-Q-TOF-MS) 的检测方法。方法 采用Waters Acquity BEH C18色谱柱(2.1 mm×100 mm,1.7 μm), 流动相为乙腈-甲酸-水体系梯度洗脱,流速为0.45 mL· min-1,质谱正离子模式扫描,进样量:2.0 μL。结果 7种成分在一定范围内均呈现良好线性,r均大于0.999 6;精密度重复性和稳定性良好;加样回收率在99%～101%之间。结论 所建立的方法简便准确快速重复性好,可用于小金丸中麝香酮、次乌头碱、乌头碱、原儿茶酸、阿魏酸、藁本内酯和11-羰基-β-乙酰乳香酸7种有效成分的含量测定。
Abstract
OBJECTIVE To develop a UPLC-MS method for determination of seven components (muscone, hypaconitine, aconitine, protocatechuic acid, ferulic acid, ligustilide, 11-keto-β-acetylboswellic acid) in Xiaojin pills. METHODS The analysis was performed on a Waters Acquity BEH C18 column ( 2.1 mm×100 mm,1.7 μm) with gradient elution of the mixture of acetonitrile-water-formic acid, and the flow rate was 0.45 mL· min-1; positive MS scanning mode was used; the injection volume was 2.0 μL. RESULTS Linear relationship was obtained between the concentrations and peak areas of the seven compounds (r＞0.999 6). The average recoveries (n=6) were between 99%-101%. CONCLUSION This method is simple,accurate, and reliable to determine the contents of the seven components in Xiaojin pills for the quality control.
关键词
小金丸 /
超高效液相色谱质谱联用 /
含量 /
乌头碱 /
麝香酮
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Key words
Xiaojin pills /
UPLC-MS /
content /
aconitine /
muscone
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中图分类号：
R927
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参考文献
[1] Ch. P( 2010) Vol (中国药典2010年版. 一部). 2010:506-507.[2] WANG X, LIU X. Determination of ferulic acid in Xiaojin wan soft capsules. Chin Hosp Pharm J(中国医院药学杂志), 2007, 27(3):350-352.[3] PING Y H, MAO H M, GUAN Z Y, et al. The determination of muscone in Xiaojin pills by gas chromatography. J JX Normal Univ(江西师范大学学报), 2011, 35(3):263-265.[4] ZHAO F C, LI J, LIU S M, et al. HPTLC Fingerprint analysis of Aconitum Herbals in Xinjiang. Chin Pharm J(中国药学杂志), 2013, 48(7):512-517.[5] OU C B, SHI N N, YANG Q H, et al. Protocatechuic acid, a novel active substance against avian influenza virus H9N2 infection. PLoS One, 2014, 9(10):e111004.[6] BACANLI M, AYDIN S, TANER G, et al. The protective role of ferulic acid on sepsis-induced oxidative damage in Wistar albino rats. Environ Toxicol Pharmacol, 2014, 38(3):774-782.[7] ZHU M D, ZHAO L X, WANG X T, et al. Ligustilide inhibits microglia-mediated proinflammatory cytokines production and inflammatory pain. Brain Res Bull, 2014,230(14):150-156.[8] FEI Y Q, SUN L, CHENG X L, et al. Study on the identification of boswellic acids in olibanum by high-performance thin lyer chromatography with quadrupole time of flight mass spectrometry. Chin Pharm J(中国药学杂志), 2011, 46(20):1601-1605.[9] CHEN Z, GONG X, LU Y, et al. Enhancing effect of borneol and muscone on geniposide transport across the human nasal epithelial cell monolayer. PLoS One, 2014, 9(7):e101414.[10] LIU C X. A review of Chinese research and development on pharmacokinetics. Chin Pharm J(中国药学杂志), 2010, 45(2):81-90.
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脚注
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基金
国家自然基金青年项目(81303267);中国博士后基金一等资助项目(2014M550149)
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