Külpmann W R
J Clin Chem Clin Biochem. 1980 Jun;18(6):339-44.
A gaschromatographic procedure for the simultaneous determination of ethosuximide and valproate is presented. After addition of the two internal standards the serum sample is acidified and extracted by chloroform. 2 microliters of the organic phase is directly injected into the gaschromatograph without previous evaporation. The gaschromatographic analysis is carried out on SP 1000 under isothermal conditions without derivatisation. The coefficients of variation for the precision from day to day were 2.6% (ethosuximide) and 5.2% (valproate). In external quality control the results for both substances always differed less than one standard deviation from the mean. The detection limits (11.6 mumol/l for ethosuximide and 2.3 mumol/l for valproate) were far below the usual therapeutic range. The specificity of the method was proven by comparison of the relative retention times of about 100 drugs, the investigated antiepileptic drugs and their internal standards.
本文介绍了一种同时测定乙琥胺和丙戊酸盐的气相色谱法。加入两种内标后,将血清样品酸化并用氯仿萃取。2微升有机相无需预先蒸发即可直接注入气相色谱仪。气相色谱分析在等温条件下于SP 1000上进行,无需衍生化。日间精密度的变异系数分别为2.6%(乙琥胺)和5.2%(丙戊酸盐)。在外部质量控制中,两种物质的结果与平均值的差异始终小于一个标准差。检测限(乙琥胺为11.6μmol/L,丙戊酸盐为2.3μmol/L)远低于通常的治疗范围。通过比较约100种药物、所研究的抗癫痫药物及其内标的相对保留时间,证明了该方法的特异性。