血中毒鼠强的固相萃取和GC-NPD法测定

目的 研究人全血中毒鼠强的固相革取(SPE)。方法 用Bond Elute C18固相萃取柱萃取,GC-NPD检测,以甲基对硫磷为色谱内标(CS)。结果 全血中加标0.5μg/ml,毒鼠强回收率为92.5％,变异系数2.3％(CV,n=4)。在0.5～10μg/ml的浓度范围内,线性相关系数为0.9994。检出限(S/N=3)和定量限(S/N=10)分别为6ng/ml和20ng/ml。同一根萃取柱连续使用6次未见性能明显下降(CV=3.6%)。结论 本文方法适用于毒鼠强中毒的全血测定。

Solid phase extraction and GC-NPD for determination of tetramethylenedisulfotetramine in whole blood

Objective Develop a solid phase extraction (SPE) method for extraction of tetram-ethylenedisulfotetramine (tetramine) from whole human blood. Methods The SPE was performed with Bond Elute C18 column having a 3-mL reservoir and 250mg sorbent. Gas chromatography with nitrogen phosphorus detector (GC-NPD) was used for detection, and parathion-methyl was used as chromatographic standard (CS). Results Spiking tetramine at 0.5μg/ml level in 1ml whole blood, recovery of tetramine was 92.5% with coefficient of variation (CV) 2.3% in 4 replicate assays. The limit of detection (LOD, S/N=3) and limit of quantitation (LOQ, S/N= 10) of this compound in whole blood was 6ng/ml and 20ng/ml, respectively. The linearity correlation coefficients (R2) was 0.9994 in range of 0.5-10ng/ml concentrations. The SPE column performance did not decrease in 6 successive extractions with CV 3.5% . Conclusion The developed SPE method was solvent-saved, simpleand practical. It was suitable in determination of tetramine in whole blood in forensic or clinical practice.