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采用顶空进样和化学发光检测的气相色谱法直接测定水中的痕量二甲基亚砜。

Direct measurement of part-per-billion levels of dimethyl sulfoxide in water by gas chromatography with stacked injection and chemiluminescence detection.

机构信息

Australian Centre for Research on Separation Science (ACROSS), University of Tasmania, Hobart, Tasmania, Australia.

出版信息

J Sep Sci. 2012 Jun;35(12):1486-93. doi: 10.1002/jssc.201101087.

DOI:10.1002/jssc.201101087
PMID:22740258
Abstract

Dimethyl sulfoxide (DMSO) is a chemical of industrial significance with many important applications. DMSO is used as an industrial solvent, in drug delivery and healthcare applications, among others. Analysis of DMSO in water typically involves extensive sample preparation, enrichment, and derivatization to improve solute detectability. A novel gas chromatographic procedure has been developed for the direct measurement of trace levels of DMSO in an aqueous matrix, such as potable water. The technology utilizes stacked injection techniques for in-column solute enrichment, a precolumn to enhance solute focusing effects, and sulfur chemiluminescence detection for matrix suppression and sensitivity. A detection limit of 2 parts per billion (ppb) (v/v) of DMSO in water was attained. Relative precision of less than 7% at the concentration of 10 ppb (v/v) of DMSO was demonstrated. A correlation coefficient of 0.9988 was obtained over a range of 2 ppb (v/v) to 100 ppb (v/v). No detectable carry-over was found at the 5 ppb (v/v) level whereas less than 4% carry-over was observed at the 100 ppb (v/v) level. Various sample storage media including glass, polyethylene, and polycarbonate were also studied to minimize solute loss. Recoveries greater than 84% were achieved with all storage media tested. The method was found to be reliable and simple to implement.

摘要

二甲基亚砜(DMSO)是一种具有许多重要应用的工业重要化学品。DMSO 用作工业溶剂、药物输送和医疗保健应用等。水中 DMSO 的分析通常需要进行广泛的样品制备、富集和衍生化,以提高溶质的可检测性。本文开发了一种新的气相色谱程序,用于直接测量水基基质(如饮用水)中痕量 DMSO。该技术利用柱内溶质富集的堆叠进样技术、增强溶质聚焦效果的预柱和硫化学发光检测,用于基质抑制和灵敏度。在水中达到 2 十亿分比浓度(ppb)(v/v)的 DMSO 检测限。在 10 ppb(v/v)DMSO 浓度下,相对精度小于 7%。在 2 ppb(v/v)至 100 ppb(v/v)的范围内,获得了 0.9988 的相关系数。在 5 ppb(v/v)水平下未发现可检测的夹带,而在 100 ppb(v/v)水平下观察到的夹带小于 4%。还研究了各种样品储存介质,包括玻璃、聚乙烯和聚碳酸酯,以尽量减少溶质损失。用所有测试的储存介质均实现了大于 84%的回收率。该方法可靠且易于实施。

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