Külpmann W R
J Clin Chem Clin Biochem. 1979 Feb;17(2):89-96.
A simple gas chromatographic method for the determination of commercially available barbiturates used as hypnotics is presented. Saturated ammonium sulfate is added to the serum sample. The mixture is extracted three times with chloroform. The organic layer is dried over sodium sulfate and evaporated. The residue is dissolved in ethyl acetate/acetic acid (100 ml + 1 ml) and an aliquot is injected into the gas chromatograph. The precision in the series is between 3.0 and 7.2%; the recovery--with the exception of propallylonal--between 91 and 108%; the detection limit from 1.7 to 6.9 mumol/l. The specificity of the method was checked by comparing 1) the results obtained before and after additional purification of the extract by thin-layer chromatography, and 2) the retention times of about 100 drugs in the gas chromatographic systems that are used.
本文介绍了一种用于测定市售用作催眠药的巴比妥类药物的简单气相色谱法。向血清样品中加入饱和硫酸铵。混合物用氯仿萃取三次。有机层用硫酸钠干燥并蒸发。残留物溶于乙酸乙酯/乙酸(100 ml + 1 ml),取一份注入气相色谱仪。该系列中的精密度在3.0%至7.2%之间;回收率(除烯丙异丙巴比妥外)在91%至108%之间;检测限为1.7至6.9 μmol/l。通过比较以下两项来检验该方法的特异性:1)提取物经薄层色谱进一步纯化前后获得的结果;2)约100种药物在所用气相色谱系统中的保留时间。