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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Development and application of a rapid and sensitive LC-MS/MS method for simultaneous quantification of six diterpene lactones in rats after oral administration of Rhizoma Dioscoreae Bulbiferae extract
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Development and application of a rapid and sensitive LC-MS/MS method for simultaneous quantification of six diterpene lactones in rats after oral administration of Rhizoma Dioscoreae Bulbiferae extract

机译：快速敏感LC-MS / MS法的开发和应用，用于口服六磷瘤大鼠大鼠六次二萜内酯的血管基

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Diterpene lactones have been considered as the main therapeutic and hepatotoxic constituents of Rhizome Dioscoreae Bulbiferae in recent years. In this work, a simple, rapid and accurate LC-MS/MS method was established and validated to determine six diterpene lactones in rat plasma simultaneously, including Diosbulbin B (DIOB), Diosbulbin C (DIOC), Diosbulbin D (DIOD), Diosbulbin G (DIOG), Diosbulbin J (DIOJ) and Diosbulbin L (DIOL), after oral administration of Rhizoma Dioscoreae Bulbiferae extract. The six diterpene lactones, with the inclusion of two pairs of isomer (DIOB & D, DIOC & L), and Buspirone (internal standard, IS) were successfully separated using an XDB-C-18 column with the gradient elution, consisting of water with 0.1% (v/v) FA and methanol with 0.1% (v/v) FA, under a flow rate of 0.50 mL/min in 5.8 min. Precursor-product ion transitions were optimized to be m/z 362.1 -> 317.1, 363.1 -> 207.1, 345.0 -> 299.2, 364.3 -> 347.0, 396.3 -> 379.3, 363.2 -> 345.1 and 386.3 -> 122.2 for DIOB, DIOC, DIOD, DIOG, DIOJ, DIOL and buspirone at positive ion mode with an electrospray ionization source (ESI), respectively. The linearity ranges of this present method were 0.50 to 500 mu g/L for DIOB, 20.0 to 20,000 mu g/L for DIOC and 2.00 to 2000 mu g/L for DIOD, DIOG, DIOJ and DIOL, respectively. And the LLOQs were as low as 0.20 mu g/L for DIOB, 20.0 mu g/L for DIOC and 2.00 mu g/L for DIOB, D, G, J and L. The accuracy of each analyte was within the range of 95.8% to 101.0% and the precision was < 11.3%. No matrix effect and carry over was observed, and the recovery of the six analytes ranged from 87.3% to 109% with the RSD < 11.4% within the concentrations range. The validated method was further applied to the pharmacokinetics investigation of DIOB, DIOC, DIOD, DIOG, DIOJ and DIOL successfully after oral administration of Rhizoma Dioscoreae Bulbiferae extract at 1.53 g/kg in rates.
机译：近年来，二萜内酯被认为是根茎二十甲孢子菌的主要治疗性和肝毒性成分。在这项工作中，建立并验证了一种简单，快速和精确的LC-MS / MS方法，以同时测定大鼠血浆中的六个二萜内酯，包括Diosbulbin B（DioB），Diosbulbin C（DIOC），Diosbulbin D（Diod），Diosbulbin G（二焦），DioSbulbin J（DIOJ）和Diosbulbin L（二醇），原子施用后咪昔粒子蛋白提取物。使用XDB-C-18柱包含两对异构体（DiOB＆D，DioC＆L）和BusPirone（内标，Queal标准）的六个二萜内酯和BusPirone（内标是）的梯度洗脱成功分离在5.8分钟内，0.1％（v / v）Fa和0.1％（v / v）Fa的Fa，流速为0.50ml / min。前体 - 产物离子转变被优化为M / Z 362.1 - > 317.1,363.1 - > 207.1,345.0 - > 299.2,364.3 - > 347.0,396.3 - > 379.3,363.2 - > 345.1和386.3 - > 122.2为DIOB，DIOC ，Diod，DioG，DIOJ，二醇和BusPirone分别具有电喷雾电离源（ESI）的正离子模式。本发明方法的线性范围分别为DIOB的0.50至500μg/ L，用于DIOC，DIOC，DIOJ和二醇的DIOC和2.00至2000μg/ L.对于DIOB，LLOQ对DIOB的0.20μg/ L低至0.20μmg/ l，对于DIOB，D，G，J和L.每分析物的准确度为95.8 ％〜101.0％，精度<11.3％。没有观察到基质效应和携带，并且六分析物的回收率范围为87.3％至109％，浓度范围内的RSD <11.4％。验证的方法进一步应用于DiOB，DIOC，DIOD，DioG，DIOJ和二醇的药代动力学调查在口服施用Rhizoma Dioscoreae Bulbiferae提取物以1.53g / kg以1.53g / kg的速率。

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