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采用稳定同位素稀释液相色谱/电喷雾电离串联质谱法测定人血清中的地高辛。

Determination of digoxin in human serum using stable isotope dilution liquid chromatography/electrospray ionization-tandem mass spectrometry.

作者信息

Mitamura Kuniko, Horikawa Aki, Yamane Yuko, Ikeda Yukari, Fujii Youichi, Shimada Kazutake

机构信息

Division of Pharmaceutical Sciences, Graduate School of Natural Science and Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan.

出版信息

Biol Pharm Bull. 2007 Sep;30(9):1653-6. doi: 10.1248/bpb.30.1653.

Abstract

A method for the determination of digoxin in human serum using a liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) technique is reported. Digoxin and the internal standard, [21,21,22-(2)H(3)]digoxin, were extracted from 250 mul of human serum using a solid phase extraction cartridge (Oasis HLB) and analyzed by LC/ESI-MS/MS in the selected reaction monitoring mode. The intra- and inter-assay reproducibility and accuracy were satisfactory within the quantification range of 0.20-3.20 ng/ml. The concentrations of digoxin in the serum samples obtained from digitalized patients (n=19) were in the range of 0.25-2.84 ng/ml, which were compared to those obtained by radioimmunoassay.

摘要

报道了一种使用液相色谱/电喷雾电离串联质谱(LC/ESI-MS/MS)技术测定人血清中地高辛的方法。地高辛和内标[21,21,22-(2)H(3)]地高辛采用固相萃取柱(Oasis HLB)从250μl人血清中萃取,并在选择反应监测模式下通过LC/ESI-MS/MS进行分析。在0.20 - 3.20 ng/ml的定量范围内,批内和批间的重现性及准确性令人满意。从接受洋地黄化治疗的患者(n = 19)获取的血清样本中地高辛浓度在0.25 - 2.84 ng/ml范围内,并与放射免疫分析法所得结果进行了比较。

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