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建立了土壤和水体中20种除草剂残留的气相色谱-质谱(GC-MS)分析方法。土壤样本通过乙腈提取,Florisil固相萃取柱净化,V(石油醚)∶V(乙酸乙酯)=9∶1洗脱,GC-MS测定;水体样本用C18固相萃取柱进行富集和净化,以V(甲醇)∶V(乙酸乙酯)=1∶1洗脱,GC-MS测定。20种除草剂在土壤和水体中的平均添加回收率分别为72%～109%和77%～113%,相对标准偏差(RSD)分别在0.15%～16.5%和0.45%～16.3%之间,方法定量限(LOQ)在土壤中为0.01 mg/kg,在水体中为0.1μg/L。用所建方法可同时检测土壤和水中20种常用除草剂,方法净化效果好、灵敏度高、重现性好、简便快速。
A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 20 herbicides in soil and water. Soil samples were extracted by acetonitrile, purified by Florisil solid phase extraction column, eluted with V (petroleum ether): V (ethyl acetate) = 9: 1 and determined by GC-MS. Water samples were enriched and purified by C18 solid phase extraction , Eluting with V (methanol): V (ethyl acetate) = 1: 1, and determined by GC-MS. The average recoveries of 20 herbicides in soil and water ranged from 72% to 109% and from 77% to 113%, respectively, and the relative standard deviations (RSDs) ranged from 0.15% to 16.5% and from 0.45% to 16.3% Method The limit of quantitation (LOQ) was 0.01 mg / kg in soil and 0.1 μg / L in water. The established method can simultaneously detect 20 common herbicides in soil and water, and has the advantages of good purification effect, high sensitivity, good reproducibility, quick and easy operation.