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A Screening Method for Cyanide in Blood by Dimethoxytriazinyl Derivatization-GC/MS
Journal of Chromatographic Science ( IF 1.5 ) Pub Date : 2020-11-05 , DOI: 10.1093/chromsci/bmaa081
Akinori Yamaguchi 1 , Hajime Miyaguchi 1
Affiliation  

A simple screening analysis of cyanide in blood has been developed, using 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (DMTMM). DMTMM, a convenient reagent for dehydrocondensation, converted cyanide to 2-cyano-4,6-dimethoxy-1,3,5-triazine, the dimethoxytriazinyl derivative of cyanide. This reaction proceeded in whole blood samples after treatment with trichloroacetic acid, and in basic aqueous solution samples. Sufficient sensitivity was observed by the method using gas chromatography/mass spectrometry. Intra- and inter-day repeated analyses (0.05, 0.1, 0.25, 1 and 5 μg/mL, n = 5) were performed and the accuracy and precision were within 20% for the lower limit of quantification (LLOQ) and within 15% for other concentrations. LLOQs for the aqueous solution and blood were 0.05 and 0.1 μg/mL, respectively, which are suitable for detecting cyanide poisoning. The limits of detection (signal-to-noise ratio ≥ 3) for aqueous solution and blood were 0.01 and 0.05 μg/mL, respectively. Interference from 13 other anions was tested and no false positive response was obtained, even in the case of thiocyanate, nitrite and nitrate, which are known to yield cyanide by acid treatment of blood. This method is practical because it uses readily available reagents and equipment and is sensitive enough for the rapid screening of cyanide poisoning in forensic and clinical toxicology.

中文翻译:

二甲氧基三嗪基衍生化-GC / MS筛选血液中氰化物的方法

使用4-(4,6-二甲氧基-1,3,5-三嗪-2-基)-4-甲基吗啉氯化物(DMTMM),开发了一种简单的血液中氰化物筛选分析方法。DMTMM是一种方便的脱氢试剂,将氰化物转化为2-氰基-4,6-二甲氧基-1,3,5-三嗪,氰化物的二甲氧基三嗪基衍生物。该反应在用三氯乙酸处理后的全血样品中和碱性水溶液样品中进行。通过使用气相色谱/质谱的方法观察到足够的灵敏度。日内和日间重复分析(0.05、0.1、0.25、1和5μg/ mL,n = 5),对于定量下限(LLOQ),准确度和精密度在20%以内,对于其他浓度,准确度和精密度在15%以内。水溶液和血液的LLOQ分别为0.05和0.1μg/ mL,适用于检测氰化物中毒。水溶液和血液的检出限(信噪比≥3)分别为0.01和0.05μg/ mL。测试了来自其他13种阴离子的干扰,即使在已知通过血液酸处理产生氰化物的硫氰酸盐,亚硝酸盐和硝酸盐的情况下,也未获得假阳性反应。该方法是实用的,因为它使用了现成的试剂和设备,并且足够灵敏,可以快速筛查法医和临床毒理学中的氰化物中毒。
更新日期:2020-12-17
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