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采用毛细管气相色谱法和高效液相色谱法分析正己烷、2-己酮、2,5-己二酮及相关化学品。

Analysis of n-hexane, 2-hexanone, 2,5-hexanedione, and related chemicals by capillary gas chromatography and high-performance liquid chromatography.

作者信息

Nomeir A A, Abou-Donia M B

出版信息

Anal Biochem. 1985 Dec;151(2):381-8. doi: 10.1016/0003-2697(85)90192-7.

Abstract

Analytical methods, using capillary gas chromatography and normal-phase high-performance liquid chromatography, were developed for the analysis of the neurotoxic chemicals n-hexane, 2-hexanone, and 2,5-hexanedione and their suspected metabolites. Two gas chromatographic methods, using a 50-m glass capillary OV 101 column and cyclohexane as an internal standard, were employed. In both methods, the injector and detector temperatures were 220 and 280 degrees C, respectively. In method I the following temperature program was used: isothermic at 50 degrees C for 30 min, followed by a temperature increase of 10 degrees C/min to a final temperature of 180 degrees C, which was then maintained for 7 min. This method was used to analyze the following compounds: n-hexane, 2,5-dimethylfuran, 2-hexanone, 3-hexanone, hexanal, 1-hexanol, 2-hexanol, 3-hexanol, 5-hydroxy-2-hexanone, gamma-valerolactone, 2,5-hexanedione, and 2,5-hexanediol. Method II, which was developed for n-hexane and eight of its more common metabolites, used the following temperature program: isothermic at 70 degrees C for 15 min, followed by a temperature increase of 40 degrees C/min to a final temperature of 220 degrees C, which was maintained for 5 min. A linear relationship between peak area and amount injected was observed over a 100-fold range. The minimum detectable amounts ranged from 0.05 to 1 microgram, depending on the compound. Normal-phase HPLC, using a 5-micron silica cartridge fitted into an RCM-100 radial-compression separation system, was utilized to analyze 2-hexanone and its metabolites 2,5-dimethylfuran, gamma-valerolactone, 5-hydroxy-2-hexanone, and 2,5-hexanedione.(ABSTRACT TRUNCATED AT 250 WORDS)

摘要

开发了采用毛细管气相色谱法和正相高效液相色谱法的分析方法,用于分析神经毒性化学物质正己烷、2-己酮、2,5-己二酮及其疑似代谢产物。采用了两种气相色谱法,使用一根50米长的玻璃毛细管OV 101柱,以环己烷作为内标。在这两种方法中,进样器和检测器温度分别为220℃和280℃。方法I采用以下温度程序:50℃等温30分钟,然后以10℃/分钟的速率升温至最终温度180℃,并保持7分钟。该方法用于分析以下化合物:正己烷、2,5-二甲基呋喃、2-己酮、3-己酮、己醛、1-己醇、2-己醇、3-己醇、5-羟基-2-己酮、γ-戊内酯、2,5-己二酮和2,5-己二醇。方法II是针对正己烷及其八种更常见的代谢产物开发的,采用以下温度程序:70℃等温15分钟,然后以40℃/分钟的速率升温至最终温度220℃,并保持5分钟。在100倍的范围内观察到峰面积与进样量之间呈线性关系。根据化合物的不同,最低检测量范围为0.05至1微克。采用正相高效液相色谱法,使用安装在RCM - 100径向压缩分离系统中的5微米硅胶柱,用于分析2-己酮及其代谢产物2,5-二甲基呋喃、γ-戊内酯、5-羟基-2-己酮和2,5-己二酮。(摘要截取自250字)

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