Norwegian Defence Research Establishment (FFI), PO Box 25, NO-2027 Kjeller, Norway.
J Chromatogr A. 2010 Jan 29;1217(5):761-7. doi: 10.1016/j.chroma.2009.12.008. Epub 2009 Dec 4.
A method for trace determination of sulphur mustard (HD) and some of its cyclic decomposition compounds in water samples has been developed using headspace-trap in combination with gas chromatography-mass spectrometry (GC-MS). Factorial design was used for optimisation of the method. The trap technology allows enrichment and focusing of the analytes on an adsorbent, hence the technique offers better sensitivity compared to conventional static headspace. A detection limit of 1ng/ml was achieved for HD, while the cyclic sulphur compounds 1,4-thioxane, 1,3-dithiolane and 1,4-dithiane could be detected at a level of 0.1ng/ml. The method was validated for the stable cyclic compounds in the concentration range from the limit of quantification (LOQ: 0.2-0.4ng/ml) to hundred times LOQ. The within and between assay precisions at hundred times LOQ were 1-2% and 7-8% relative standard deviation, respectively. This technique requires almost no sample handling, and the total time for sampling and analysis was less than 1h. The method was successfully employed for muddy river water and sea water samples.
已开发出一种使用顶空捕集结合气相色谱-质谱联用（GC-MS）测定水样中硫芥（HD）及其一些环状分解化合物的痕量方法。使用析因设计对方法进行了优化。捕集技术允许在吸附剂上对分析物进行富集和聚焦，因此与传统的静态顶空相比，该技术具有更好的灵敏度。HD 的检测限达到 1ng/ml，而环状硫化合物 1,4-噻烷、1,3-二硫戊环和 1,4-二噻烷可在 0.1ng/ml 的水平下检测到。该方法已针对稳定的环状化合物在从定量下限（LOQ：0.2-0.4ng/ml）到 100 倍 LOQ 的浓度范围内进行了验证。在 100 倍 LOQ 时，日内和日间测定精密度分别为 1-2%和 7-8%相对标准偏差。该技术几乎不需要样品处理，采样和分析的总时间不到 1 小时。该方法已成功用于泥泞河水和海水样品。
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