摘要
目的:建立一种同时测定中毒者血样中25种有机磷农药和鼠药的固相萃取净化GC/MS方法.方法:血样中加入异丙威内标物,丙酮提取有机磷农药和毒鼠强,采用Oasis HLB固相小柱净化,用毛细柱气相色谱分离,采用选择离子监测(SIM)的质谱扫描模式进行定量分析.结果:25种有机磷农药和毒鼠强检出限为 20～30 ng/ml,定量限为 60～90 ng/ml,血样加标 100～1 000 ng/ml 的平均回收率为 48.9%～98.9%,重复测定6次的RSD值小于 10%,血样中OPs在加入EDTA二钠盐后在 -20℃条件下保存稳定.结论:该方法具有较高的灵敏度、准确度和精密度,可满足血样中有机磷农药和毒鼠强快速检测分析的要求.
Objective ： To develop a rapid and sensitive method for the simultaneous determination of 25 organophosphorus pesticides and tetramine in blood and serum samples, using a combination of rapid Oasis HLB cartridges solid - phase extraction and capillary gas chromatography with mass spectrometric detection. Methods： The OPs and tetramine in serum or blood samples were extracted with acetone after addition of internal standard isoprocarb and then cleaned up by Oasis HLB SPE. The eluate was analyzed by selected ion monitoring mode using GC/MS. Results： Extraction recoveries of 25 OPs and tetramine in a 100 - 1 000 ng/ ml spiked blood and serum samples ranged between 48.9% and 98. 9%. The limit of detection and limit of quantitation ranged from 20 to 30 ng/ml and from 60 to 90 ng/ml,respectively. The RSD was satisfactory with less than 10%. OPs in blood or serum samples proved to be stable at - 20~C after addition of EDTA salt. Conclusion： The method is sensitive, accurate and precise for rapid determination of 25 OPs and tetramine in blood and serum samples and meets the requirements of biological monitoring of exposure to OPs and tetramine.
出处
《中国卫生检验杂志》
CAS
2005年第9期1025-1029,共5页
Chinese Journal of Health Laboratory Technology
基金
深圳市医疗卫生科技计划项目(200405225)
