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超高效液相色谱-四极杆-线性离子阱质谱联用同时测定五味子中木脂素类和有机酸类成分

[Simultaneous determination of lignans and organic acids in Schisandrae Chinensis Fructus by UFLC-Q-TRAP-MS/MS].

作者信息

Chen Shu-Yu, Shi Jing-Jing, Zou Li-Si, Liu Xun-Hong, Tang Ren-Mao, Ma Ji-Mei, Yan Ying, Zhao Hui

机构信息

School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.

SZYY Group Pharmaceutical Limited, Taizhou 225500, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2018 May;43(10):2104-2111. doi: 10.19540/j.cnki.cjcmm.20180115.019.

Abstract

An analytical method based on UFLC-QTRAP-MS/MS was developed for simultaneous determination of fifteen components including eleven lignans (schizantherin B, schisandrol B, schizandrin C, γ-schisandrin, deoxyschizandrin, schisantherin, schisandrin, schisanhenol, gomisin D, gomisin J, and angeloylgomisin H) and organic acids (S)-malic acid, D(-)-tartaric acid, protocatechuic acid, and quinic acid) in Schisandrae Chinensis Fructus. Samples from different product specifications were evaluated and analyzed. The chromatographic separation was performed on a Synergi™ Hydro-RP 100Å column (2.0 mm×100 mm, 2.5 μm) at 40 °C with a gradient elution by employing 0.1% aqueous formic acid (A)-acetonitrile (B) as the mobile phase, and the flow rate was 0.4 mL·min⁻¹, using an electrospray ionization (ESI) source and multiple reaction monitoring (MRM) mode. Fifteen components were evaluated synthetically by TOPSIS and gray related degree. The results showed that fifteen components had good linearity (r>0.999 90), and the limits of detection were all satisfactory. The average recoveries of standard addition for the compounds were between 95.42 % and 98.86 %, and the relative standard deviations were less than 5%. The greatest difference of ri in grey related degree was 58.1%, whilst the greatest difference of Ci value in TOPSIS method was 94.8%. The results of these two methods showed that the holistic quality of No. 14 sample was the best. The developed method was accurate and reliable, which was suitable for the simultaneous determination of multiple functional substances and able to provide a new basis for the comprehensive assessment and overall control of the quality of Schisandrae Chinensis Fructus.

摘要

建立了一种基于超高效液相色谱-串联四极杆线性离子阱质谱(UFLC-QTRAP-MS/MS)的分析方法,用于同时测定五味子果实中的15种成分,包括11种木脂素(南五味子素B、五味子醇B、五味子酯甲、γ-五味子素、去氧五味子素、南五味子宁、五味子醇甲、五味子酚、戈米辛D、戈米辛J和当归酰戈米辛H)和有机酸(S)-苹果酸、D(-)-酒石酸、原儿茶酸和奎尼酸)。对不同产品规格的样品进行了评估和分析。色谱分离在Synergi™ Hydro-RP 100Å柱(2.0 mm×100 mm,2.5μm)上于40℃进行,采用梯度洗脱,以0.1%甲酸水溶液(A)-乙腈(B)为流动相,流速为0.4 mL·min⁻¹,采用电喷雾电离(ESI)源和多反应监测(MRM)模式。采用逼近理想解排序法(TOPSIS)和灰色关联度对15种成分进行综合评价。结果表明,15种成分线性关系良好(r>0.999 90),检测限均令人满意。化合物的标准加入平均回收率在95.42%至98.86%之间,相对标准偏差小于5%。灰色关联度中ri的最大差值为58.1%,而TOPSIS法中Ci值的最大差值为94.8%。这两种方法的结果表明,14号样品的整体质量最佳。所建立的方法准确可靠,适用于多种功能成分的同时测定,能够为五味子果实质量的综合评价和全面控制提供新的依据。

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