Department of Pharmacy, School of Stomatology, Fourth Military Medical University, Xi'an, P. R. China.
J Sep Sci. 2012 Sep;35(17):2203-9. doi: 10.1002/jssc.201200393. Epub 2012 Jul 19.
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.
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。