CAJ | 학술논문

采用乙酸-乙腈溶液(体积比1：99)超声提取,乙二胺-N-丙基硅烷和十八烷基硅烷键合硅胶吸附剂进行分散固相萃取净化,建立了气相色谱-电子捕获法(GC-ECD),用该方法检测了土壤中甲氰菊酯、高效氯氟氰菊酯、氯菊酯、氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯7种拟除虫菊酯类农药残留。结果显示,7种拟除虫菊酯类农药在0.004~2.000 mg/L范围内农药浓度与峰面积线性关系良好；7种农药在0.01~0.50 mg/kg添加水平下,平均回收率为91.6%~100.3%,相对标准偏差为1.3%~9.8%,检出限为0.0018~0.0088 mg/kg,定量限为0.0290~0.0058 mg/kg。将该方法应用于16份茶园土壤样品中7种拟除虫菊酯类农药的残留测定,其中4份样品含有高效氯氟氰菊酯,含量为0.0075~0.0134 mg/kg,1份样品含有氟氯氰菊酯,含量为0.038 mg/kg。该方法操作简单、结果准确、溶剂用量少、分析成本低,可以满足土壤中拟除虫菊酯类农药的检测需要。
채용을산-을정용액(체적비1：99)초성제취,을이알-N-병기규완화십팔완기규완건합규효흡부제진행분산고상췌취정화,건립료기상색보-전자포획법(GC-ECD),용해방법검측료토양중갑청국지、고효록불청국지、록국지、불록청국지、록청국지、청무국지、추청국지7충의제충국지류농약잔류。결과현시,7충의제충국지류농약재0.004~2.000 mg/L범위내농약농도여봉면적선성관계량호；7충농약재0.01~0.50 mg/kg첨가수평하,평균회수솔위91.6%~100.3%,상대표준편차위1.3%~9.8%,검출한위0.0018~0.0088 mg/kg,정량한위0.0290~0.0058 mg/kg。장해방법응용우16빈다완토양양품중7충의제충국지류농약적잔류측정,기중4빈양품함유고효록불청국지,함량위0.0075~0.0134 mg/kg,1빈양품함유불록청국지,함량위0.038 mg/kg。해방법조작간단、결과준학、용제용량소、분석성본저,가이만족토양중의제충국지류농약적검측수요。
A gas chromatograph-electron captured detection( GC-ECD) method was developed for simultaneous deter-mination of fenpropathrin, lambda-cyhalothrin, permethrin, cyfluthrin, cypermethrin, fenvalerate and deltamethrin in soil based on the ultrasound assisted extraction of the sample with acetic acid-acetonitrile solution ( volume ratio,1 : 99 ) as sol-vent and the following purification by dispersive solid phase extraction ( DSPE) using PSA ( primary secondary amine) and C18 ( octadecylsilane bonded silica) as adsorbents. Good linearities between concentrations and peak areas were achieved in the concentration range of 0. 004-2. 000 mg/L for target pesticides, with correlation coefficients higher than 0. 999. The aver-age recoveries of target pesticides in soil were 91. 6%-100. 3% with the relative standard deviations ranging from 1. 3% to 9. 8% in the spiked level of 0. 01-0. 50 mg/kg. The limits of detection (LOD) by means of matrix-matched external standard method for target pyrethroid pesticides were 0. 001 8-0. 008 8 mg/kg and the limits of quantification ( LOQ) were 0. 029 0-0. 005 8 mg/kg. The method was employed to detect the 7 pyrethroid pesticides residues in the soil collected from local tea garden in Suzhou. Among 16 soil samples, lambda-cyhalothrin was detected in 4 samples with the content varying from 0. 007 5 to 0. 013 4 mg/kg, and cyfluthrin was detected in one sample with the content of 0. 038 mg/kg. This method is simple, accurate, solvent saving and cost saving, and provides an easy way to simultaneously determine the pyre-throid pesticides in soil.