Seto Y, Tsunoda N, Ohta H, Shinohara T
National Research Institute of Police Science, Tokyo, Japan.
J Anal Toxicol. 1993 Nov-Dec;17(7):415-20. doi: 10.1093/jat/17.7.415.
Headspace (HS) capillary gas chromatography with flame-ionization detection was developed for the determination of chloroform levels in blood. Separation of chloroform was improved significantly using a DB-WAX capillary column, without interference by other volatile substances. Sensitivity was increased by adjusting the splitter ratio to 20, without any decline in peak resolution. The HS conditions, a 50 degrees C incubation for 30 min, gave reproducible and sensitive determinations. The distribution coefficient (k) was calculated to be 8.24. The CV was 1.8% for 27.7 micrograms/mL chloroform, and the detection limit was 0.02 microgram/mL (S/N = 4) when the splitter ratio was 10. Raising HS temperature resulted in a significant decrease in k for chloroform in the absence of blood, in contrast to the relatively small effect seen in the presence of blood. Although inorganic salts showed a salting-out effect, erythrocytes and hydrophobic compounds, such as detergent and lipid, significantly suppressed the vaporization of chloroform. Chloroform was found to be distributed mainly in erythrocytes when incubated with blood overnight at 2 degrees C.
建立了顶空（HS）毛细管气相色谱-火焰离子化检测法用于测定血液中的氯仿水平。使用DB-WAX毛细管柱可显著改善氯仿的分离效果，且不受其他挥发性物质的干扰。通过将分流比调整为20提高了灵敏度，同时峰分辨率没有任何下降。顶空条件为50℃孵育30分钟，可实现可重复且灵敏的测定。计算得出分配系数（k）为8.24。当氯仿浓度为27.7微克/毫升时，变异系数（CV）为1.8%，当分流比为10时，检测限为0.02微克/毫升（信噪比=4）。在没有血液存在的情况下，提高顶空温度会导致氯仿的k值显著降低，而在有血液存在时，这种影响相对较小。尽管无机盐表现出盐析效应，但红细胞以及去污剂和脂质等疏水化合物会显著抑制氯仿的汽化。当在2℃下与血液过夜孵育时，发现氯仿主要分布在红细胞中。
