分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
12期
1378-1383
,共6页
陈猛%陆婉清%韩燕%黄群腾%孙广大
陳猛%陸婉清%韓燕%黃群騰%孫廣大
진맹%륙완청%한연%황군등%손엄대
农药%河水%海水%固相萃取%气相色谱
農藥%河水%海水%固相萃取%氣相色譜
농약%하수%해수%고상췌취%기상색보
pesticide%river water%sea water%solid phase extraction%gas chromatography
应用固相萃取和气相色谱技术建立了河水和海水中36种常用农药(7种有机氯、11种有机磷、8种拟除虫菊酯、4种酰胺、2种苯胺和4种唑类杂环)的分析方法.采用Oasis HLB柱为水样富集萃取柱,考察了洗脱溶剂、上样体积、pH值和离子强度等因素对萃取效果的影响,采用无水硫酸钠和NH2柱进行除水和净化.目标农药在0.9 ~2 600 μg/L范围内线性良好;以PCB103为内标物,2,4,5,6-四氯间二甲苯、环氟菌胺和氟丙菊酯为替代物,实际河水、海水的加标回收率分别为62% ~124%、64% ~132%,相对标准偏差(n=3)分别为0.2% ~9.6%、0.1% ~12.2%;方法检出限为0.10 ~1.0 ng/L.方法快速、灵敏、准确,已成功应用于福建九龙江入海口表层水样的分析.
應用固相萃取和氣相色譜技術建立瞭河水和海水中36種常用農藥(7種有機氯、11種有機燐、8種擬除蟲菊酯、4種酰胺、2種苯胺和4種唑類雜環)的分析方法.採用Oasis HLB柱為水樣富集萃取柱,攷察瞭洗脫溶劑、上樣體積、pH值和離子彊度等因素對萃取效果的影響,採用無水硫痠鈉和NH2柱進行除水和淨化.目標農藥在0.9 ~2 600 μg/L範圍內線性良好;以PCB103為內標物,2,4,5,6-四氯間二甲苯、環氟菌胺和氟丙菊酯為替代物,實際河水、海水的加標迴收率分彆為62% ~124%、64% ~132%,相對標準偏差(n=3)分彆為0.2% ~9.6%、0.1% ~12.2%;方法檢齣限為0.10 ~1.0 ng/L.方法快速、靈敏、準確,已成功應用于福建九龍江入海口錶層水樣的分析.
응용고상췌취화기상색보기술건립료하수화해수중36충상용농약(7충유궤록、11충유궤린、8충의제충국지、4충선알、2충분알화4충서류잡배)적분석방법.채용Oasis HLB주위수양부집췌취주,고찰료세탈용제、상양체적、pH치화리자강도등인소대췌취효과적영향,채용무수류산납화NH2주진행제수화정화.목표농약재0.9 ~2 600 μg/L범위내선성량호;이PCB103위내표물,2,4,5,6-사록간이갑분、배불균알화불병국지위체대물,실제하수、해수적가표회수솔분별위62% ~124%、64% ~132%,상대표준편차(n=3)분별위0.2% ~9.6%、0.1% ~12.2%;방법검출한위0.10 ~1.0 ng/L.방법쾌속、령민、준학,이성공응용우복건구룡강입해구표층수양적분석.
A method for simultaneous determination of 36 pesticides(7 organochlorines,11 organophosphorous,8 pyrethrins,4 amides,2 nitrodiphenylamines and 4 heterozoles) in river water and sea water was established by combination of solid phase extraction and gas chromatography(SPE/GC).Oasis HLB cartridge was selected to extract and enrich target pesticides.Effect of experimental conditons,such as elution solvents,loading speed,penetration volume,cleanup cartridges,pH and salinity on extraction efficiency were investigated.Under the optimized conditions,the calibration curves showed good linearity between 0.9 and 2 600 μg/L for targeted compounds.With PCB103 as internal standard,2,4,5,6-tetrachloro-m-xylene,cyflufenamid and acrinathrin as surrogates,recoveries of 36 pesticides from river water and sea water at two spiking levels were in the range of 62%-124% and 64%-132%,respectively,their relative standard deviations(n=3) were 0.2%-9.6% and 0.1%-12.2%,respectively.Method detection limits ranged from 0.10 to 1.0 ng/L.The method was fast,sensitive,accurate,and was successfully applied in the analysis of pesticide in surface waters of Jiulong River estuary,Fujian province.