梭曼异构体气相色谱分析及在小鼠脑及膈肌中的浓度测定

Gas chromatographic analysis of the stereoisomers of soman in mice brain and diaphragm

目的 :建立灵敏、可靠的梭曼光学异构体气相分析方法以测定小鼠皮下染毒后脑与膈肌中游离梭曼的浓度。方法 :大进样量气相色谱仪及手性毛细管柱实现梭曼 4个异构体的分离 ;用二异丙基氟磷酸酯作内标 ,测定小鼠皮下染毒后脑与膈肌中游离C(± )P(- )梭曼。结果 :梭曼 4个异构体在确定的气相条件下得到了较好的分离 ;C(± )P(- )梭曼在小鼠脑匀浆中及膈肌匀浆中 ,0 .5～ 10ng/ 2ml浓度范围的标准曲线线性关系良好 ,r >0 .999。日间、日内精密度在 10 %以内 ,提取方法的回收率为 5 3.6%～ 60 .2 %。用气相色谱分析方法考察了小鼠皮下染毒后 ,脑与膈肌中游离C(± )P( )梭曼的浓度 ,方法重复性好。结论 :大进样量气相色谱仪及手性毛细管柱测定小鼠皮下染毒后脑与膈肌中游离C(± )P(- )梭曼的浓度 ,方法灵敏、可靠 。

Objective:To establish a method for determination of the concentration of the stereoisomers of soman in mice brain and diaphragm after soman was subcutaneously administrated to mice.Methods:Chiral capillary gas chromatographic analysis method with large volume injections was used to separate the stereoisomers of soman. After subcutaneous administration,the concentration of C(±)P(-)soman was determined by using DFP as internal standard.Results:The four stereoisomers of soman were well separated by the chiral capillary gas chromatographic column. The linearity of the calibration curves was good( r >0.999) when the concentration range of C(±)P(-)soman in mouse brain and diaphragm homogenate was 0.5-10?ng/2?ml. The precision was within 10% and average percentage extraction recovery ranged from 53.6 to 60.2%. The concentration of C(±)P(-)soman in mouse brain and diaphragm determined by chromatographic analysis method had good repeatability. Conclusions:Gas chromatographic analysis method which measures the concentration of the stereoisomers of soman in mouse brain and diaphragm after subcutaneous administration is sensitive, reliable and has good repeatability.