单甲脒和2,4-二甲基苯胺在大鼠肝脏中的残留分析

DETERMINATION OF N'- (2, 4-DIMETHYLPHENYD-N-METHYLFORMAMIDINE AND 2,4-DIMETHYLAMINE RESIDUES IN RAT LIVER

本文研究了大鼠肝脏中单甲脒及其代谢产物2.4-二甲基苯胺残留量的气相色谱分析方法.肝脏匀浆用1mol·1^(-1)HCl加热回流提取,等分为A,B两份,A份溶液调pH至13后用石油醚萃取定容;B份加两倍体积的10mol·1^(-1)NaOH 溶解后用石油醚萃取定容.分别经七氟丁酸酐衍生化,用带电子捕获检测器的气相色谱仪测定2,4-二甲基苯胺的含量,最后计算单甲脒的残留量.该方法对2,4-二甲基苯胺的最低检出浓度为0.25×10^(-11)g,回收率80%,相对误差小于2%,相对标准偏差小于6%,能同时测定样品中单甲脒和2,4-二甲基本胺的含量.

Determination of N'- ( 2, 4- dimethylphenyl )- N- methylformamidine (DMA) and 2,4-dimethylamine (DMB) residues in rat liver by gas chromatography (GC) was described. Liver samples were extracted with 1mol : 1-1 HC1 following homogenzing; the acid extracts were equally divided into A and B two parts. The pH of part A was adjusted to 13, part B was hydrolyzed with adding two volumes of 10mol· 1-1 NaOH solution and heating reflux; both A and B were extracted with petroleum ether and derivated with heptafluorobutyric anhydride separately. The concentration of DMB was determined by GC and DMA was calculated. The minimum detection limit is less than 0. 25×10-11g with the relative error of 2% and the relative standard deviation of 6%. The recovery is 80%. DMA and DMB in sample can be determined simultaneously by the method.