Ye H P, Shao J, Tan S W, Shan X Y, Shi Y P
Hangzhou Occupational Disease Prevention and Control Hospital, Hangzhou 310014, China.
Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2017 Oct 20;35(10):780-782. doi: 10.3760/cma.j.issn.1001-9391.2017.10.020.
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. 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(30m×0.32mm×0.15μm)and detected byECD.The retention time was for qualitative analysis and the internal standard was for quantitation. The standard curves of TCE and TCOH showed significant linearity between 95.5μg/L-7640.0μg/L(=0.9997)and 19.0μg/L-1520.0μg/L(=0.9992). The average recovery was 95.5%-103.6%.The intra-day and inter-day precisions()were 2.5%-6.8%(=6)and 1.6%-4.3%(=6) respectively. The detect limit of TCE and TCOH were 2.10 μg/L and 0.56μg/L(S/N=3)respectively.The blood can be kept 7 days at-20℃ refrigerator without significantly loss. 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.
建立一种液液萃取-气相色谱-电子捕获检测器法测定血样中三氯乙烯(TCE)和三氯乙醇(TCOH)的方法。采用该方法,以乙醚为萃取溶剂,三氯甲烷为内标。全血样品用乙醚萃取,经无水硫酸钠脱水。然后在HP-5毛细管柱(30m×0.32mm×0.15μm)上分离分析物,用电子捕获检测器检测。以保留时间定性,以内标法定量。TCE和TCOH的标准曲线在95.5μg/L - 7640.0μg/L(r = 0.9997)和19.0μg/L - 1520.0μg/L(r = 0.9992)范围内呈良好线性。平均回收率为95.5% - 103.6%。日内和日间精密度(RSD)分别为2.5% - 6.8%(n = 6)和1.6% - 4.3%(n = 6)。TCE和TCOH的检测限分别为2.10μg/L和0.56μg/L(S/N = 3)。血样在-20℃冰箱中可保存7天,无明显损失。该方法简便、实用、灵敏度高,能满足TCE接触者血样测定的要求。