中国中药杂志

2014, v.39(12) 2345-2350

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UPLC-MS/MS同时测定大承气汤大鼠血浆中9种活性成分的含量
Simultaneous determination of 9 major components of Dachengqi Tang in rat plasma by UPLC-MS/MS

申峰云;魏惠珍;孙勇兵;王跃生;吕尚;高萌;曾恋情;饶毅;
SHEN Feng-yun;WEI Hui-zhen;SUN Yong-bing;WANG Yue-sheng;LV Shang;GAO Meng;ZENG Lian-qing;RAO Yi;Jiangxi University of Chinese Traditional Medicine;The National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;

摘要(Abstract):

该研究建立了大鼠血浆中大承气汤9种活性成分同时测定的UPLC-MS/MS方法。采用Aglient C18色谱柱(2.1mm×50 mm,1.7μm)进行色谱分离,利用甲醇-5 mmol·L-1甲酸铵流动相进行梯度洗脱,流速0.3 mL·min-1。实验过程血浆的前处理不仅考察了甲醇、乙腈等有机溶剂蛋白沉淀法,同时考察了液-液萃取法中不同萃取溶剂、不同涡旋时间、萃取次数及不同体积萃取溶剂等因素对各活性成分回收率的影响。最终确定以布洛芬为内标,采用乙酸乙酯液-液萃取法进行血样前处理,N2吹干复溶,离心后上清液进行UPLC-MS/MS分析,在电喷雾电离(ESI)负离子模式下,采用多重反应监测模式进行检测。大黄素、大黄酸、芦荟大黄素、大黄素甲醚、大黄酚、厚朴酚、和厚朴酚、橙皮苷及橙皮素的线性范围分别为0.33~660,0.40~792,0.41~827,0.34~680,0.45~907,0.46~927,0.43~867,0.34~683,0.39~787μg·L-1,且线性关系良好;提取回收率均>69.39%;日内和日间的RSD<15%。该方法符合生物样品分析的要求,可用于研究大鼠灌胃大承气汤后,血浆中该9种活性成分的同时测定,为其量-效物质基础提供了理论依据。
The study established a UPLC-MS/MS method that is used for simultaneous determination nine major bioactive compounds of Dachengqi Tang in rat plasma. Using Aglient C18column(2. 1 mm ×50 mm,1. 7 μm) was chromatographed,using methanol-5 mmol·L-1ammonium formate mobile phase gradient,elution 0. 3 mL·min-1. In the plasma pre-treatment process,not only the method of methanol and acetonitrile protein precipitation was investigated,and different factors extraction solvent,the type of the scroll time,the number and the type of extraction solvent,the extraction volume of the extraction solution of liquid-liquid extraction is investigated. Finally,with ibuprofen as an internal standard,using ethyl acetate liquid-liquid extraction method pretreatment blood,N2dry reconstituted supernatant after centrifugation UPLC-MS/MS analysis,in electrospray ionization(ESI) negative mode,using multiple reaction monitoring mode for testing. The linear range of emodin,rhein,aloe-emodin,chrysophanol,magnolol,honokiol,hesperidin and hesperitin is 0. 33-660,0. 40-792,0. 41-827,0. 34-680,0. 45-907,0. 46-927,0. 43-867,0. 34-683,0. 39-787 μg·L-1respectively,good linear relationship; and extraction recovery were greater than69. 39%,days after the day of the RSD is less than 15%. This method can be used to study the rat gastric large bearing gas after Dachengqi Tang,the simultaneous determination of nine components in plasma for its pharmacokinetics and efficacy material base to provide a theoretical basis.

关键词(KeyWords): UPLC-MS/MS;大承气汤;血药浓度
UPLC-MS/MS;Dachengqi Tang;blood drug concentration

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基金项目(Foundation): 国家重点基础研究发展计划(973)项目(2010CB530602)

作者(Author): 申峰云;魏惠珍;孙勇兵;王跃生;吕尚;高萌;曾恋情;饶毅;
SHEN Feng-yun;WEI Hui-zhen;SUN Yong-bing;WANG Yue-sheng;LV Shang;GAO Meng;ZENG Lian-qing;RAO Yi;Jiangxi University of Chinese Traditional Medicine;The National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;

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