土壤和水体中20种除草剂的气相色谱-质谱法多残留分析  

Multiresidue analysis of 20 herbicides in soil and water by gas chromatography-mass spectrometry

作　　者：王铁龙[1] 胡继业[1] 

机构地区：[1]北京科技大学化学与生物工程学院,北京100083

出　　处：《农药学学报》2012年第6期629-634,共6页Chinese Journal of Pesticide Science

摘　　要：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 rapid multiresidue method has been developed for the simultaneous analysis of 20 herbicides in soil and water by gas chromatography-mass spectrometry（GC-MS）.Residues were extracted from soil with acetonitrile,purified by solid phase extraction（SPE）,eluted by V（petroleum ether）∶V（ethyl acetate）=9∶1 and then concentrated to a small volume with acetone before GC-MS analysis.The target compounds in water were extracted with C18 SPE and eluted by V（methanol）∶V（ethyl acetate） =1 ∶1.The average recoveries of 20 herbicides ranged from 72%-109% in soil with relative standard deviations（RSDs） 0.15%-16.5% and 77%-113% in water with the RSDs 0.45%-16.3%,respectively.The limits of quantification（LOQs） were 0.01 mg/kg in soil and 0.1 μg/L,respectively.The results indicated that the developed method is sensitive,reproducible and has good cleanup effect.

关 键 词：气相色谱-质谱 土壤 水体 除草剂 残留 

分 类 号：O657[理学—分析化学] X52[理学—化学]