Determination of cyanide in whole blood by capillary gas chromatography with cryogenic oven trapping
Determination of cyanide in whole blood by capillary gas chromatography with cryogenic oven trapping
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DOI：
10.1021/ac980498b
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发表时间：
1998-11-15
影响因子：
7.4
通讯作者：
Kumazawa, T
中科院分区：
文献类型：
--
作者：
Ishii, A;Seno, H;Kumazawa, T
氰化物是一种重要的有毒物质，采用毛细管气相色谱法（GC），在顶空（HS）进样的条件下，用低温炉捕集，可以高灵敏度地测定氰化物。HS样品中的全部氰化物可以在在线GC分析之前被低温捕获，在存在或不存在氰化物和丙腈的情况下，0.5mL体积的血液（内标，IS）加入到含有0.25 mt蒸馏水、0.3 g Na（2）SO（4）、0.2 mt 50%H（3）PO（4）和0.1g抗坏血酸（当需要时），并将混合物在70 ℃下加热15 min。将5 mL体积的HS蒸气引入GC毛细管柱中：在无分流模式下，在-30 ℃烘箱温度下，将其编程至160 ℃，用于具有氮-磷检测的GC分析。在本条件下，氰化物得到一个尖锐的峰，背景非常干净。氰化物和IS的萃取效率分别为2.89-3.22（100或500 ng/mL）和2.42%。日内和日间变异系数分别为2.9和11.8%，实际火灾受害者血中氰化物含量平均值为687 ± 597 ng/mL（mean +/- SD，n = 9）。健康受试者的内源性血氰化物浓度为8.41 +/- 3.09 ng/mt（平均值+/- SD，n = 6）。
Cyanide, one of the most important toxic substances, has been found measurable with high sensitivity by capillary gas chromatography (GC) with cryogenic oven trapping upon injection of headspace (HS) vapor samples. The entire amount of cyanide in the HS sample could be cryogenically trapped prior to on-line GC analysis, A 0.5mL volume of blood in the presence or absence of cyanide and propionitrile (internal standard, IS) was added to a vial containing 0.25 mt of distilled water, 0.3 g of Na(2)SO(4), 0.2 mt of 50% H(3)PO(4), and 0.1 g of ascorbic acid (when needed), and the mixture was heated at 70 degrees C for 15 min. A 5-mL volume of the HS vapor was introduced into a GC capillary column:in the splitless mode at -30 degrees C oven temperature that was programmed up to 160 degrees C for GC analysis with nitrogen-phosphorus detection. A sharp peak was obtained for cyanide under the present conditions, and backgrounds were very clean. The extraction efficiencies of cyanide and IS were 2.89-3.22 (100 or 500 ng/mL) and 2.42%, respectively. The calibration curve showed good linearity in the range of 25-1000 ng/mL and the detection limit was similar to 2 ng/mL, The coefficients of intraday and interday variations were 2.9 and 11.8%, respectively, The mean blood cyanide level measured for actual fire victims was 687 +/- 597 ng/mL,(mean +/- SD, n = 9). Endogenous blood cyanide concentration for healthy subjects was 8.41 +/- 3.09 ng/mt (mean +/- SD, n = 6).