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毛细管气相色谱-质谱法测定血浆中布新洛尔及其主要代谢物

Determination of bucindolol and its major metabolites in plasma by capillary gas chromatography-mass spectrometry.

作者信息

Bartek M J, Kerns E H, Gammans R E, Gallo D G

出版信息

J Chromatogr. 1986 Apr 25;377:183-94. doi: 10.1016/s0378-4347(00)80773-2.

Abstract

A method for determining bucindolol, a deuterated analogue and two metabolites in plasma samples is described. Analytes are obtained from plasma by liquid extraction of 1 ml of plasma at pH 10.5 with 7 ml of peroxide-free ether-hexane (4:1). Following derivatization with 50 microliters of N-methyl-N-trimethylsilyl trifluoroacetamide-pyridine (1:1) for 20 min at 65 degrees C the samples are analyzed by capillary column gas chromatography-mass spectrometry with selected-ion monitoring. Quantification is linear over the range 2-500 ng/ml. Single-day precision was typically 6.2% or better for bucindolol and 13% or better for the metabolites.

摘要

描述了一种测定血浆样品中布辛多洛、一种氘代类似物和两种代谢物的方法。通过在pH 10.5下用7 ml无过氧化物的乙醚 - 己烷(4:1)对1 ml血浆进行液液萃取从血浆中获得分析物。在65℃下用50微升N - 甲基 - N - 三甲基硅基三氟乙酰胺 - 吡啶(1:1)衍生化20分钟后,通过毛细管柱气相色谱 - 质谱联用选择离子监测对样品进行分析。定量在2 - 500 ng/ml范围内呈线性。布辛多洛的单日精密度通常为6.2%或更好,代谢物的单日精密度为13%或更好。

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