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衍生化后采用超高效液相色谱-电喷雾电离质谱法对大鼠血浆中曲坦特罗进行对映体选择性测定。

Enantioselective determination of trantinterol in rat plasma by ultra performance liquid chromatography-electrospray ionization mass spectrometry after derivatization.

作者信息

Yang Jing, Wang Yanjuan, Pan Li, Li Ning, Lu Xiumei, Guan Jin, Cheng Maosheng, Li Famei

机构信息

Department of Analytical Chemistry, Shenyang Pharmaceutical University, Shenyang, PR China.

出版信息

Talanta. 2009 Oct 15;79(5):1204-8. doi: 10.1016/j.talanta.2009.03.036. Epub 2009 Mar 26.

Abstract

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the determination of trantinterol enantiomers in rat plasma. Diphenhydramine was employed as the internal standard. The plasma samples were prepared using liquid-liquid extraction with n-hexane-dichloromethane-isopropanol (20:10:1, v/v/v) as the extractant. Trantinterol enantiomers after pre-column derivatization using diacetyl-l-tartaric anhydride (DATAAN) were separated on a C18 column using a gradient solvent programme. The mobile phase was composed of 3mM ammonium acetate and acetonitrile. The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI). Linear calibration curve for each enantiomer was obtained in the concentration range of 1-80 ng/mL, with limit of quantification (LOQ) of 1 ng/mL. The intra- and inter- precision (R.S.D.) values were below 9.6% and accuracy (R.E.) was from -2.4 to 6.2% at all quality control (QC) levels. The developed method was applied to the enantioselective pharmacokinetic study of trantinterol in rats.

摘要

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法并进行了验证,用于测定大鼠血浆中的川丁特罗对映体。采用苯海拉明作为内标。血浆样品采用正己烷-二氯甲烷-异丙醇(20:10:1,v/v/v)作为萃取剂进行液-液萃取制备。川丁特罗对映体经二乙酰-L-酒石酸酐(DATAAN)柱前衍生后,在C18柱上采用梯度溶剂程序进行分离。流动相由3mM醋酸铵和乙腈组成。通过电喷雾电离(ESI)在三重四极杆串联质谱仪上采用多反应监测(MRM)模式进行检测。各对映体在1-80 ng/mL浓度范围内获得线性校准曲线,定量限(LOQ)为1 ng/mL。在所有质量控制(QC)水平下,批内和批间精密度(R.S.D.)值均低于9.6%,准确度(R.E.)为-2.4%至6.2%。所建立的方法应用于川丁特罗在大鼠体内的对映体选择性药代动力学研究。

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