血中三氯乙烯和三氯乙醇同时测定的液液萃取-气相色谱法

Simultaneous determination of trichloroethylene and trichloroethanol in blood by liquid-liquid extraction-gas chromatography

目的建立液液萃取气相色谱法同时测定血液中三氯乙烯及其代谢物三氯乙醇。方法以三氯甲烷为内标物，乙醚为萃取剂，吸取有机相经无水硫酸钠干燥后注入气相色谱仪，经HP．5毛细管色谱柱（30m×0．32mm×0．15μm）分离，采用电子捕获检测器检测，以保留时间定性，内标法定量。结果三氯乙烯、三氯乙醇的线性范围分别为95．5～7640．0、19．0～1520．0wg／L，相关系数为0．9997、0．9992，以3倍信噪比估算方法检出限分别为2．10、0．56wg／L，两种物质样品加标回收率为95．5％～103．6％，批内、批间精密度分别为2．5％-6．8％、1．6％～4．3％。样品在-20℃冰箱中至少可以保存7d。结论该方法简单实用，重现性好，灵敏度高，可以应用于三氯乙烯职业接触人群的生物检测。

Objective To establish a method for determing the trichloroethylene（TCE） and trichloroethanol （TCOH） in blood samples by liquid-liquid extraction-gas chromatography with electron capture detector. Methods With this method, ether was used as extraction solvent and trichloromethane was used as an internal standard. The whole blood sample was extracted with ether, and dehydrated by anhydrous sodium sulfate. Then the analytes were separated on HP-5 capillary column （30 m×0.32 mm×0.15 μm） and detected by ECD. The retention time was for qualitative analysis and the internal standard was for quantitation. Results The standard curves of TCE and TCOH showed significant linearity between 95.5 ~g/L-7 640.0 μg/L（r=0.999 7） and 19.0 μg/L-1 520.0 txg/L（r=0.999 2）. The average recovery was 95.5%-103.6%. The intra-day and inter-day precisions （RSD） were 2.5%-6,8% （n=6） and 1.6%-4.3% （n=6） respectively. The detect limit of TCE and TCOH were 2.10 μg/L and 0.56 μg/L （S/N =3） respectively. The blood can be kept 7 days at -20℃ refrigerator without significantly loss. Conclusion This method is proved to be simple, practical and highly sensitive. It can satisfy the request for the determination of blood samples of humans exposed to TCE.