建立以正己烷为萃取剂的衍生化-液液萃取-气相色谱/质谱法,对水中常见6种有机锡化合物进行测定。通过考察萃取时间及pH等因素对萃取和衍生化效率的影响而对测定方法进行优化,进一步评价测定方法的检测限、精密度及准确度。结果表明,对小体积(O.2mL)水样不经过浓缩处理,采用直接萃取衍生化一GC/MS法测定有机锡化合物最低检测限可达0.42μg/L;对大体积(500mL)水样通过衍生化-萃取-浓缩过程,再经GC/MS测定有机锡化合物最低检测限可达0.11ng/L。采用该方法对水中不同浓度有机锡化合物测定的相对标准偏差〈7.7%,加标回收率为80.5%~108.0o,4。该方法可对大量的较高浓度(μg/L级)有机锡污染物水样进行快速、准确测定,同时也适用于测定痕量(ng/L级)有机锡污染的实际水体。
Liquid liquid extraction with n-hexane as extractant followed by gas chromatography/mass spectrometry(GC/MS) detection have been investigated for the speciation analysis of six organotin com- pounds in water. Factors, for examlpe of extraction time, pH value et al, were considered in order to eval- uate their influence on the efficiency of liquid liquid extraction and derivatization and optimize the analytic method. The evaluation of accuracy, precision and limits of detections(LOIN)has allowed the method to be validated, too. The results to determine the concentration of organotin compounds in water samples indicate that, the method of samples with small volume(0. 2 mL) directly derivatizated and extracted at the same time followed by GC/MS without concentration process, whose lowest LODs can reach 0. 42/μg/L. And the one of samples with large volume(500 mL)were derivatizated, then extrated and concentrated process, following with GC/MS, whose lowest LOIN can reach 0. 11 ng/L. The relative standard deviation of the method is under 7.7 %and recovery with standard addition is 80. 5 % - 108. 0 % for different water samples of oganotin compounds. These results show that the method appears to be rapid and accuracy to determi- nate the organotins in water not only with high concentration asμg/L level of massive samples but also with trace concentraion as ng/L level of real water body.