Application of ultrahigh-performance liquid chromatography coupled with mass spectrometry for analysis of lignans and quality control of Fructus Schisandrae chinensis.
Application of ultrahigh-performance liquid chromatography coupled with mass spectrometry for analysis of lignans and quality control of Fructus Schisandrae chinensis.
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DOI：
10.1002/jssc.201200393
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发表时间：
2012-09
影响因子：
3.1
通讯作者：
Wei-Dong Zhang;Qing Wang;Ying Wang;Xiao-Juan Wang;J. Pu;Yi Gu;Rong Wang
中科院分区：
文献类型：
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作者：
Wei-Dong Zhang;Qing Wang;Ying Wang;Xiao-Juan Wang;J. Pu;Yi Gu;Rong Wang
中药北五味子中的木脂素类化合物具有抗肝毒、平喘、抗胃溃疡等生物活性。建立了一种超高效液相色谱-四极杆飞行时间质谱联用方法，通过同时定性和定量分析15种木脂素来评价FSC的质量，这些木脂素包括野牡丹苷A、B和C;野牡丹醇A和B;戈米辛B、C、D、E、G、H、J和N;虎香酰戈米辛H;当归酰戈米辛H。采用Zorbax Eclipse Plus C（18）（2.1 × 100 mm，1.8 μm）色谱柱，以乙腈-0.1%甲酸为流动相进行梯度洗脱。木脂素通过其保留时间、准确的质量数据和特征离子与参比物质进行比较来鉴定。所有校准曲线在检测范围内均呈良好的线性回归（r（2）> 0.99）。进样10 μL时，所有分析物的检测限和定量限均在0.1-4 ng/mL范围内。方法的重复性（相对标准偏差<4.6%）和回收率（85.58-105.82%）均较好。同时，整个样品分析时间小于10 min，为全面评价FSC的质量提供了新的依据。
Lignans in the drug Fructus Schisandrae chinensis (FSC) exhibit potent biological activities such as antihepatotoxic, antiasthmatic, and antigastric ulcer. An ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method has been developed to evaluate the quality of FSC through simultaneous qualitative and quantitative analysis of 15 lignans, including schizandrin A, B, and C; schizandrol A and B; gomisin B, C, D, E, G, H, J, and N; tigloylgomisin H; and angeloylgomisin H. The compounds were separated on a Zorbax Eclipse Plus C(18) (2.1 × 100 mm, 1.8 μm) column with a gradient elution of acetonitrile and 0.1% formic acid. Lignans were identified through their retention times, accurate mass data, and characteristic ions by comparison with a reference substance. All calibration curves showed perfect linear regression (r(2) > 0.99) within the test range. The limits of detection and quantitation fell in the ranges of 0.1-4 ng/mL for all the analytes with an injection of 10 μL. Good results were obtained with respect to repeatability (relative standard deviation <4.6%) and recovery (85.58-105.82%). Meanwhile, the entire sample analysis time was less than 10 min. This developed method provided a new basis for the overall assessment of the quality of FSC.