UFLC-QTRAP-MS/MS同时测定五味子中木脂素及有机酸类成分
投稿时间:2017-12-08  修订日期:2017-12-27  责任编辑:  点此下载全文
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作者中文名作者英文名单位中文名单位英文名E-Mail
陈舒妤 CHEN Shu-yu 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine m18305172513@163.com 
石婧婧 SHI Jing-jing 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine  
邹立思 ZOU Li-si 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine  
刘训红* LIU Xun-hong 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine liuxunh1959@163.com 
唐仁茂 TANG Ren-mao 江苏苏中药业集团股份有限公司 SZYY Group Pharmaceutical Limited  
马继梅 MA Ji-mei 江苏苏中药业集团股份有限公司 SZYY Group Pharmaceutical Limited  
严 颖 YAN Ying 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine  
赵 慧 ZHAO Hui 南京中医药大学 School of Pharmacy,Nanjing University of Chinese Medicine
China
SZYY Group Pharmaceutical Limited
China
 
基金项目:国家中药标准化项目(ZYBZH-C-JS-32);江苏高校优势学科建设工程资助项目(YSXK-2014);江苏高校品牌专业建设工程资助项目 (PPZY2015A070)
中文摘要:建立超快速液相色谱-三重四极杆/线性离子阱质谱(UFLC-QTRAP-MS/MS)同时测定五味子中木脂素(五味子酯乙、五味子醇乙、五味子丙素、五味子乙素、五味子甲素、五味子酯甲、五味子醇甲、五味子酚、戈米辛 D、戈米辛 J、当归酰基戈米辛 H)及有机酸(L-苹果酸、酒石酸、原儿茶酸、奎宁酸)共15种指标成分含量的方法,并对其商品药材进行分析与评价。采用SynergiTM Hydro-RP 100?柱(100 mm × 2.0 mm, 2.5 μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,柱温40 ℃,流速0.4 mL·min-1?,电喷雾离子源(ESI),多反应监测离子扫描模式(MRM)测定;用灰色关联度分析结合TOPSIS法对15种目标成分进行综合评价。结果表明,15种化合物在一定浓度范围内均呈现良好的线性关系,相关系数大于0.990;精密度、重复性和稳定性良好;平均加样回收率在95.42 %~98.86 %之间,RSD均小于5 %。灰色关联度分析中ri的最大差异较小为58.1 %,TOPSIS法中Ci值的最大差异达到 94.8 %,两种综合评价结果均显示S14的综合质量最好。所建立的方法准确、可靠,可用于五味子中多元指标成分或功效物质的同时测定,为五味子药材内在质量的综合评价和全面控制提供新的方法参考。
中文关键词:五味子  超快速液相色谱-三重四极杆/线性离子阱质谱  木脂素  有机酸  含量测定
 
Simultaneous determination of lignans and organic acids in Schisandrae Chinensis Fructus by UFLC-QTRAP-MS/MS
Abstract:A comprehensive analytical method based on UFLC-QTRAP-MS/MS was developed for the simultaneous determination of fifteen components included lignans (Schizantherin B、Schisandrol B、Schizandrin C、γ-schisandrin、Deoxyschizandrin、Schisantherin、Schisandrin、Schisanhenol、Gomisin D、Gomisin J、Angeloylgomisin H) and organic acids ((S)-malic acid、D(-)-Tartaric acid、Protocatechuic acid、Quinic acid) in Schisandrae Chinensis Fructus. Samples from different product specifications were evaluated and analysed. The chromatographic separation was performed on a SynergiTM Hydro-RP 100? column (100 mm × 2.0 mm, 2.5 μm) at 40 °C with a gradient elution of 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). Fifteen components were evaluated synthetically by TOPSIS and gray related degree. The results show that fifteen components have good linearity, the linearity of the detected components is excellent more than 0.990, and the limits of detection are all satisfied. The average recoveries of standard addition for the compounds are between 95.42 % and 98.86 %, and the relative standard deviations are less than 5 %. The biggest difference of ri in grey related degree was 58.1 %, whilst the biggest difference of Ci value in TOPSIS method was 94.8 %. The result of these two methods showed that the comprehensive quality of the sample 14 was the best. The established method is accurate and reliable, which is suitable for the simultaneous determination of multiple functional substances and can provide a new basis for the comprehensive assessment and overall control of the quality of Schisandrae Chinensis Fructus.
keywords:Schisandrae Chinensis Fructus  UFLC-QTRAP-MS/MS  lignans  organic acids  quantitative determination
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