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通过液相色谱-串联质谱法测定妊娠Sprague-Dawley大鼠中莪术二酮含量的分析方法的建立与应用。

Development and application of an analytical method for curdione quantification in pregnant Sprague-Dawley rats by LC-MS/MS.

作者信息

Meng Xiang, Zhang Ting, Li Ying, Pan Qi, Jiang Juan, Luo Yongwei, Chong Liming, Yang Yang, Xu Sichong, Zhou Li, Sun Zuyue

机构信息

Pharmacy School of Fudan University, 2140 Xie Tu Road, Shanghai, People's Republic of China.

Department of Pharmacology and Toxicology, Shanghai Institute of Planned Parenthood Research, 2140 Xie Tu Road, Shanghai, 200032, People's Republic of China.

出版信息

Biomed Chromatogr. 2015 Oct;29(10):1499-505. doi: 10.1002/bmc.3449. Epub 2015 Mar 4.

DOI:10.1002/bmc.3449
PMID:25736727
Abstract

The vaginal administration route suffers from relatively low absorption efficiency, which may hinder the identification of the toxicokinetics of curdione in pregnant women. A sensitive analytical method for determining the plasma concentration of curdione was developed and applied in the determination of curdione in pregnant Sprague-Dawley rats as a simulated model. Glimepiride was used as an internal standard and chromatographic separation was achieved on a Capcell Pak C18 MGIII column. A gradient elution profile with 0.5% formic acid (A)-0.5% formic acid-acetonitrile (B) was selected as mobile phase. The selected reaction monitoring mode was used for quantification based on the target fragment ions m/z 237.2 to m/z 135.1 for curdione and m/z 491.3 to m/z 352.1 for the glimepiride. The standard curve was linear over the range of 0.5-500 ng/mL for curdione in rat plasma and yielded a consistent peak pattern, even at the lower limit of quantitation of 0.5 ng/mL. The retention times of curdione and IS were 6.55 and 6.59 min, respectively. The mean recovery of curdione in rat plasma was 95.5-101.1%. The intra-day and inter-day precisions were between 2.35 and 9.08%. This LC-MS/MS method provides a simple and sensitive means for determining the plasma concentration.

摘要

阴道给药途径的吸收效率相对较低,这可能会妨碍莪术二酮在孕妇体内毒代动力学的研究。本文建立了一种灵敏的测定血浆中莪术二酮浓度的分析方法,并将其应用于以怀孕的Sprague-Dawley大鼠为模拟模型的莪术二酮测定。以格列美脲为内标,在Capcell Pak C18 MGIII柱上实现色谱分离。选用0.5%甲酸(A)-0.5%甲酸-乙腈(B)的梯度洗脱模式作为流动相。基于莪术二酮的目标碎片离子m/z 237.2至m/z 135.1以及格列美脲的目标碎片离子m/z 491.3至m/z 352.1,采用选择反应监测模式进行定量分析。大鼠血浆中莪术二酮的标准曲线在0.5-500 ng/mL范围内呈线性,即使在定量下限0.5 ng/mL时也能产生一致的峰型。莪术二酮和内标的保留时间分别为6.55和6.59分钟。大鼠血浆中莪术二酮的平均回收率为95.5-101.1%。日内和日间精密度在2.35%至9.08%之间。这种液相色谱-串联质谱法为测定血浆浓度提供了一种简单而灵敏的方法。

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