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固相萃取-气相色谱-质谱联用快速测定水中的1,4-二氧六环

Rapid determination of 1,4-dioxane in water by solid-phase extraction and gas chromatography-mass spectrometry.

作者信息

Song D, Zhang S

机构信息

Clinical Research Associates, New York, NY 10010, USA.

出版信息

J Chromatogr A. 1997 Nov 7;787(1-2):283-7. doi: 10.1016/s0021-9673(97)00661-4.

Abstract

A highly sensitive and accurate gas chromatography-mass spectrometry method for rapidly quantitative analysis of dioxane in water samples is described. Dioxane in water sample was extracted by hexane-methylene chloride (80:20, v/v) then transferred to a C18 solid-phase extraction (SPE) cartridge and eluted by acetonitrile. An aliquot of this solution was analyzed by gas chromatography-mass spectrometry with electron impact ionization and selected ion monitoring (dioxane m/z 88) mode. The quantitative limit was set to be 0.05 microgram/ml with an injection volume of 2 microliters and a sample volume of 1 ml. The isotopically labelled [2H8]dioxane (m/z 96) was used as internal standard. Analysis time is approximately 6 min. The results for various kinds of SPE cartridges in this method are also discussed.

摘要

描述了一种用于快速定量分析水样中二恶烷的高灵敏度和准确的气相色谱 - 质谱法。水样中的二恶烷用己烷 - 二氯甲烷(80:20,v/v)萃取,然后转移至C18固相萃取(SPE)柱并以乙腈洗脱。取该溶液的一份等分试样,采用电子轰击电离和选择离子监测(二恶烷m/z 88)模式通过气相色谱 - 质谱法进行分析。在进样体积为2微升且样品体积为1毫升的情况下,定量限设定为0.05微克/毫升。使用同位素标记的[2H8]二恶烷(m/z 96)作为内标。分析时间约为6分钟。还讨论了该方法中各种SPE柱的结果。

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