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Simultaneous determination of cyanide and thiocyanate in plasma by chemical ionization gas chromatography mass-spectrometry (CI-GC-MS)

机译:化学电离气相色谱质谱法(CI-GC-MS)同时测定血浆中氰化物和硫氰酸盐

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An analytical method utilizing chemical ionization gas chromatography-mass spectrometry was developed for the simultaneous determination of cyanide and thiocyanate in plasma. Sample preparation for this analysis required essentially one-step by combining the reaction of cyanide and thiocyanate with pentafluorobenzyl bromide and simultaneous extraction of the product into ethyl acetate facilitated by a phase-transfer catalyst, tetrabutylammonium sulfate. The limits of detection for cyanide and thiocyanate were 1 μM and 50 nM, respectively. The linear dynamic range was from 10 μM to 20 mM for cyanide and from 500 nM to 200 μM for thiocyanate with correlation coefficients higher than 0.999 for both cyanide and thiocyanate.The precision, as measured by %RSD, was below 9 %, and the accuracy was within 15 % of the nominal concentration for all quality control standards analyzed. The gross recoveries of cyanide and thiocyanate from plasma were over 90 %. Using this method, the toxicokinetic behavior of cyanide and thiocyanate in swine plasma was assessed following cyanide exposure.
机译:建立了一种利用化学电离气相色谱-质谱法同时测定血浆中氰化物和硫氰酸盐的分析方法。用于该分析的样品制备基本上需要一个步骤,将氰化物和硫氰酸盐与五氟苄基溴的反应合并,并在相转移催化剂硫酸四丁铵的作用下,将产物同时萃取到乙酸乙酯中。氰化物和硫氰酸盐的检出限分别为1μM和50 nM。氰化物的线性动态范围为10μM至20 mM,硫氰酸盐的线性动态范围为500 nM至200μM,氰化物和硫氰酸盐的相关系数均高于0.999。%RSD测得的精密度低于9%,并且对于所有分析的质量控制标准,准确度均在标称浓度的15%以内。血浆中氰化物和硫氰酸盐的总回收率超过90%。使用这种方法,在接触氰化物后评估了猪血浆中氰化物和硫氰酸盐的毒代动力学行为。

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