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超高效液相色谱-质谱联用分析五味子木脂素及五味子药材质量控制

Application of ultrahigh-performance liquid chromatography coupled with mass spectrometry for analysis of lignans and quality control of Fructus Schisandrae chinensis.

机构信息

Department of Pharmacy, School of Stomatology, Fourth Military Medical University, Xi'an, P. R. China.

出版信息

J Sep Sci. 2012 Sep;35(17):2203-9. doi: 10.1002/jssc.201200393. Epub 2012 Jul 19.

Abstract

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.

摘要

五味子中的木脂素具有显著的生物活性,如抗肝毒性、抗哮喘和抗胃溃疡。本研究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,用于通过同时定性和定量分析 15 种木脂素(包括五味子甲素、五味子乙素和五味子丙素;五味子醇甲和五味子醇乙;戈米辛 B、C、D、E、G、H、J 和 N;五味子酯 H 和五味子酯 H)评估五味子的质量。采用 Zorbax Eclipse Plus C(18)(2.1 × 100mm,1.8μm)柱进行分离,以乙腈和 0.1%甲酸为流动相进行梯度洗脱。通过与对照品比较保留时间、精确质量数据和特征离子对化合物进行鉴定。所有校准曲线在测试范围内均表现出良好的线性关系(r²>0.99)。所有分析物的检测限和定量限均为 10μL 进样量时,浓度在 0.1-4ng/mL 范围内。重复性(相对标准偏差<4.6%)和回收率(85.58-105.82%)均取得了良好的结果。同时,整个样品分析时间小于 10min。该方法为全面评估五味子的质量提供了新的依据。

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