【作者】 李永新；

【导师】 孙成均；

【作者基本信息】 四川大学 ， 劳动卫生与环境卫生学， 2005， 硕士

【摘要】 本文建立了同时测定蔬菜水果中12种农药的反相高效液相色谱分析方法。12种农药分别是:二嗪农、氧化乐果、甲基对硫磷、稻丰散、辛硫磷、二甲戊乐灵、甲氰菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯、氟胺氰菊酯和氯菊酯。分析方法:将样品捣碎,用乙酸乙酯超声提取,经Florisil固相萃取柱净化、正己烷—二氯甲烷（1:1,v/v）洗脱、氮气吹干浓缩、甲醇定容后用高效液相色谱柱分离、紫外检测,外标法峰面积定量。还对色谱柱选择、流动相组成及比例、流动相流速、柱温和紫外检测波长等试验条件进行优化,确定了最佳分析条件。色谱柱:phenomenex（USA）,C18,5μm,250×4.6mm;柱温:25℃;流动相:乙腈—水;流速:1.2ml/min;洗脱梯度:0～10.00min内乙腈由50%缓慢上升至64%,再在10.00min～10.01min内快速上升至67%,10.01～35.00min内乙腈由67%缓慢上升至94%。采用波长切换,在0～10.00min波长为200nm,10.00～13.00 min波长为272nm,13.00～16.00min波长为230nm,16.00～22.00min波长为289nm,22.00～25.80min波长为238nm,其余时间波长为206nm。12种农药标准曲线的相关系数范围为0.9985-0.9999;相对标准差（RSD）为0.99%～6.85%;检测限为0.14～2.65×10^-3mg/kg;在水果中加标平均回收率65.9%-103.0%,蔬菜中为62.8%-111.5%。 用本文建立的方法成功地测定了白菜、莲白、黄瓜、苹果和梨等40份样更多还原

【Abstract】 In this study, a high performance liquid chromatographic method for the simultaneous determination of 12 pesticides in vegetable and fruit samples was developed and evaluated. The 12 pesticides were: diazinon, omethoate, parathion-methyl , phenthoate , phoxim , pendimethalin , fenpropathion cypermethrin, deltamethrin, fenvalerate, fluvalinate, permethrin. The analytical procedure involved in ultrasonic extraction with ethyl acetate, purification using a Florisil SPE(solid phase extraction)column (6ml,1000mg) and n-hexane-dichloromethane(l:l,v/v). The elute fraction was blown to driness under the stream of nitrogen and the residue was dissolved in 0.10ml of methanol, followed by separation and quantitative analysis by reverse phase HPLC using gradient elution for the baseline separation of the 12 pesticides and programmed ultraviolet wavelength shift detection in 32min. Ethyl acetate was selected as extraction solvent. The chromatographic conditions, including column temperature,mobile phase,flow rate and ultraviolet detection wavelength were investigated. The optimized chromatographic conditions were: analytical column, phenomenex C18, 5μm, 250×4.6mm; column temperature, 25℃; mobile phase, acetonitrile-water; flow rate, 1.2ml/min; gradient elution from 0 min at 50% acetonitrile-water to 10min at 64% acetonitrile-water, from 10.00 min at 64% acetonitrile-water sharply to 10.01min at 67%, finally at 10.01min changed into 94% acetonitrile until35.00min when returned to 50% of acetonitrile-water.Wavelength shifts were adopted to achieve most sensitive ultraviolet wavelength for lower resolution paired peaks. We set the ultraviolet wavelength at 200nm at the beginning, and switched to 272nm at lO.OOmin, then 230nm at 13.00min, 289nm at 16.00min, 238nm at 22.00nm, and finally 206nm at 25.80min. The detection limit of the method was 2.65ug/kg for diazinon, 0.14ug/kg for omethoate, 0.73 ug/kg for parathion-methyl, 1.19fag/kg for phenthoate, 0.88ug/kg for phoxim,0.39ug/kg for pendimethalin, 0.29 ug/kg for fenpropathion, 0.50ug/kg for cypermethrin, O.38ug/kg for deltamethrin, 0.33ug/kg for fenvalerate, 0.23 ug/kg for fluvalinate, and 0.30 ug/kg for permethrin respectively. The relative standard deviations ranged from 0.99% to 6.85%. The average recoveries for the spiked fruit samples ranged from 65.9%-103.0%, and for the spiked vegetables from 62.8% to 111.5%. The method was applied to determining vegetables and fruit in total of 40 samples. It was concluded that this method was rapid, accurate, sensitive and repeatable for the determining trace pesticides in vegetable samples and fruit samples更多还原