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An LC-MS/MS Method for Simultaneous Determination of the Toxic and Active Components of Cortex Periplocae in Rat Plasma and Application to a Pharmacokinetic Study

机译:LC-MS / MS方法同时测定大鼠血浆中皮层有毒和有效成分的方法及其在药代动力学研究中的应用

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摘要

A sensitive and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine the toxic and other active components including isovanillin, scopoletin, periplocin, periplogenin, and periplocymarin after oral administration of cortex periplocae extract to rats. Plasma samples were prepared by protein precipitation with methanol. All compounds were separated on a C18 column with gradient elution using acetonitrile and formic acid aqueous solution (0.1%, v/v) as the mobile phase at a flow rate of 0.3 mL/min. The detection of all compounds was accomplished by multiple-reaction monitoring (MRM) in the positive electrospray ionization mode. The LC-MS/MS method exhibited good linearity for five analytes. The lower limit of quantification (LLOQ) was 0.48 ng/mL for scopoletin, periplogenin, and periplocymarin; 2.4 ng/mL for isovanillin and periplocin. The extraction recoveries of all compounds were more than 90% and the RSDs were below 10%. It was found that the absorption of scopoletin and periplocin was rapid in vivo after oral administration of cortex periplocae extract. Furthermore, periplocymarin possessed abundant plasma exposure. The results demonstrated that the validated method was efficiently applied for the pharmacokinetic studies of isovanillin, scopoletin, periplocin, periplogenin, and periplocymarin after oral administration of cortex periplocae extract.
机译:开发并验证了一种灵敏且简单的液相色谱-串联质谱(LC-MS / MS)方法,可在口服皮质皮质类固醇浸膏提取至体内后同时测定有毒物质和其他活性成分,包括异香兰素,东pole碱,periprocin,periplogenin和peripcycymarin。大鼠。通过用甲醇沉淀蛋白质来制备血浆样品。使用乙腈和甲酸水溶液(0.1%,v / v)作为流动相,以0.3 mL / min的流速通过梯度洗脱在C18色谱柱上分离所有化合物。所有化合物的检测均通过正电喷雾电离模式下的多反应监测(MRM)完成。 LC-MS / MS方法对五种分析物表现出良好的线性。草素,periplogenin和peripycymarin的定量下限(LLOQ)为0.48 ng / mL;异香草醛和periporcin的浓度为2.4 ng / mL。所有化合物的提取回收率均超过90%,RSD低于10%。口服皮质骨膜提取物后,发现大麦草碱和骨膜粘膜素在体内的吸收很快。此外,骨膜上皮素具有丰富的血浆暴露。结果表明,经验证的方法可有效地应用于口服皮质皮层提取物后的异香草醛,大麦草素,粘膜白蛋白,粘膜白蛋白和粘膜泛素的药代动力学研究。

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