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以稳定同位素标记的维拉帕米为内标,采用质量碎片分析法测定人血浆中的维拉帕米。

Determination of verapamil in human plasma by mass fragmentography using stable isotope-labelled verapamil as internal standard.

作者信息

Spiegelhalder B, Eichelbaum M

出版信息

Arzneimittelforschung. 1977;27(1):94-7.

PMID:576822
Abstract

In the present investigation a mass fragmentographic procedure for the quantitative determination of verapamil in human plasma was developed which makes use of the principle of mass spectrometry and of isotopic dilution: a known amount of isotopically labelled standard ([13C, 2H2]-verapamil) is added to the plasma sample. After an effective extraction procedure the ratio of the main fragments of verapamil (m/e 303) and the labelled standard (m/e 306) is measured by mass fragmentography. The lower limit of detection is at 1 ng/ml for plasma and at 10 pg/injection for pure verapamil. The precision was found to be between 3.4% and 14.4%, depending on the range (32.7 ng/ml and 2.2 ng/ml, resp.) of the concentration of verapamil in plasma.

摘要

在本研究中,开发了一种利用质谱原理和同位素稀释法对人血浆中维拉帕米进行定量测定的质量碎片分析法:向血浆样品中加入已知量的同位素标记标准品([13C, 2H2]-维拉帕米)。经过有效的萃取程序后,通过质量碎片分析法测量维拉帕米主要碎片(m/e 303)与标记标准品(m/e 306)的比例。血浆的检测下限为1 ng/ml,纯维拉帕米的检测下限为10 pg/进样。根据血浆中维拉帕米浓度范围(分别为32.7 ng/ml和2.2 ng/ml),精密度在3.4%至14.4%之间。

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