CAJ | 학술논문

对土壤中14种有机氯农药的超声提取技术和磺化、固相萃取小柱两种净化方法进行系统研究.结果表明,超声提取节省提取时间,提高分析效率;磺化法和固相萃取小柱法都有净化作用,但磺化法使样品中的艾氏剂、狄氏剂和异狄氏剂全部损失;固相萃取小柱净化当丙酮-正已烷淋洗液体积比为1:9、淋洗液收集8 mL时回收率>90%,干扰最小.方法检出限为0.63～2.59 μg/kg,精密度(RSD,n=7)为1.17%～14.66%,基体加标平均回收率为82.78%～106.94%.方法用于生态地球化学调查评价批量土壤样品的实际分析,检测结果满足评价工作需要.
대토양중14충유궤록농약적초성제취기술화광화、고상췌취소주량충정화방법진행계통연구.결과표명,초성제취절성제취시간,제고분석효솔;광화법화고상췌취소주법도유정화작용,단광화법사양품중적애씨제、적씨제화이적씨제전부손실;고상췌취소주정화당병동-정이완림세액체적비위1:9、림세액수집8 mL시회수솔>90%,간우최소.방법검출한위0.63～2.59 μg/kg,정밀도(RSD,n=7)위1.17%～14.66%,기체가표평균회수솔위82.78%～106.94%.방법용우생태지구화학조사평개비량토양양품적실제분석,검측결과만족평개공작수요.
In this paper sample pretreatment techniques including ultrasonic extraction and decontamination techniques of sulfonation and solid phase extraction (SPE) for determination of organochlorine pesticided in soil samples by gas chromatography were presented. The results show that ultrasonic extraction could save the sample treatment time and improve the efficiency of sample analysis. And both of the sulfonation and SPE provide better decontamination effect. But aldrin, dieldrin and endrin in the samples would be lost when sulfonation method was used. Under the optimized condition of acetone/n-hexane = 1 : 9 and using 8 mL leaching solution in SPE decontamination, the recovery of the analytes was better than 90% and with less interference. Detection limits of the method for organochlorine pesticides were 0.63～2.59 μg/kg and average recovery was 82.78%～106.94% with precision of 1.17%～14.66% RSD (n=7). The method has been successfully applied to the determination of organochlorine pesticides in soil samples in Eco-geochemical Investigation and Assessment Program.