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采用气相色谱/氢火焰离子化检测器同时测定偏苯三酸酐及其偏苯三酸杂质。

Simultaneous determination of trimellitic anhydride and its trimellitic acid impurity by GC/FID.

作者信息

Rushing L G, Althaus J R, Thompson H C

出版信息

J Anal Toxicol. 1982 Nov-Dec;6(6):290-3. doi: 10.1093/jat/6.6.290.

DOI:10.1093/jat/6.6.290
PMID:7162138
Abstract

Trimellitic anhydride has widespread usage in a variety of industrial processes. Inhalation of the airborne dust and fumes generated by these processes is the primary route of occupational exposure leading to a variety of respiratory maladies. Because of its extensive industrial usage and limited toxicological data, trimellitic anhydride was scheduled for toxicological evaluation. Analytical purity certification and chemical characterization of the chemical were required as prerequisites for such toxicological tests. Therefore, a sensitive and specific procedure for the analysis of trimellitic anhydride and its trimellitic acid impurity in admixture was developed. After methylation with diazomethane, the compounds were assayed by gas chromatography using flame ionization detection. Chromatography on 5% SP-2100 yielded two well separated peaks, which were used for quantitation of the parent compounds. Confirmational identity of trimellitic anhydride was determined by direct insertion probe mass spectrometry, while that of the anhydride methyl derivative and trimellitic acid trimethyl derivative was determined by gas chromatography-mass spectrometry.

摘要

偏苯三酸酐在各种工业过程中有着广泛的用途。吸入这些过程产生的空气中的粉尘和烟雾是职业接触的主要途径,会导致多种呼吸系统疾病。由于其广泛的工业用途和有限的毒理学数据,偏苯三酸酐被安排进行毒理学评估。该化学品的分析纯度认证和化学表征是此类毒理学测试的先决条件。因此,开发了一种灵敏且特异的方法来分析偏苯三酸酐及其混合物中的偏苯三酸杂质。用重氮甲烷甲基化后,使用火焰离子化检测通过气相色谱法对化合物进行测定。在5% SP - 2100上进行色谱分析产生了两个分离良好的峰,用于母体化合物的定量。偏苯三酸酐的确认性鉴定通过直接插入探针质谱法进行,而酸酐甲基衍生物和偏苯三酸三甲基衍生物的鉴定则通过气相色谱 - 质谱法进行。

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