Determination of cresol isomers and phenol in human body fluids by capillary gas chromatography with cryogenic oven trapping
Determination of cresol isomers and phenol in human body fluids by capillary gas chromatography with cryogenic oven trapping
复制标题
DOI：
10.1081/al-120014998
复制
发表时间：
2002-01-01
影响因子：
2
通讯作者：
Sato, K
中科院分区：
文献类型：
--
作者：
Lee, XP;Kumazawa, T;Sato, K
建立了毛细管气相色谱法测定人体体液中邻甲酚、间甲酚、对甲酚和苯酚的新方法。将含有四种化合物和2,4-二甲基苯酚作为内标的全血或尿液样本放入7.5毫升的小瓶中，在100度下加热10分钟后，将5ml的顶空蒸汽吸入气密注射器中。在0℃的烤箱温度下，所有蒸汽通过气相色谱仪的进样口以无分裂模式进入alpha-DEX 120中孔毛细管柱，以捕获化合物；将烘箱温度设定为170℃，用气相色谱火焰电离检测法检测。在本条件下，化合物的峰明显，各峰分离良好，全血和尿样的背景杂质含量低。回归方程在1 ~ 10 μ g 0.5 mL（-1）范围内呈良好的线性关系，r值为0.9983 ~ 0.9998。检测限（信噪比=3）为0.3 ~ 0.5马克杯0.5 mL（-1）。全血和尿样日内和日间精密度均不大于11.6%。本文还报道了口服甲酚皂液后大鼠全血中对甲酚和间甲酚的实际测定结果。
A new method for determination of o-, m- and p-cresols and phenol in human body fluids by capillary gas chromatography (GC) has been developed using cryogenic oven trapping. After heating a whole blood or urine sample containing the four compounds and 2,4-dimethylphenol as internal standard in a 7.5 mL-vial at 100degreesC for 10 min, 5 mL of headspace vapor was drawn into a gastight syringe. All vapor was introduced through an injection port of a GC instrument in the splitless mode into an alpha-DEX 120 middle-bore capillary column at 0degreesC of oven temperature for trapping the compounds; the oven temperature was programmed up to 170degreesC for their detection by GC with flame ionization detection. The present conditions gave sharp peaks for the compounds, a good separation of each peak and low background impurities for whole blood and urine samples. The regression equations for all compounds showed good linearity in the range of 1-10 mug 0.5 mL(-1), with r values of 0.9983-0.9998, for both samples. The detection limits (signal-to-noise ratio=3) for the compounds were 0.3-0.5 mug 0.5 mL(-1) for whole blood and urine samples. Intra- and inter-day precisions were not greater than 11.6%, for whole blood and urine samples. The data obtained from actual determination of p- and m-cresols in rat whole blood after oral administration of saponaceous cresol solution are also presented.