超声辅助液相微萃取-气相色谱法检测饮用水中有机磷农药残留  

Determination of Three Organophosphorus Pesticides with Ultrasound-assisted Liquid Phase Microextraction Combined with Gas Chromatography Flame Photometric Detection

作　　者：赵文婷[1] 魏朝俊[1] 贾临芳[1] 吴昆明[1] 梁丹[1] 赵建庄[1] 

机构地区：[1]北京农学院农产品有害微生物及农残安全检测与控制北京市重点实验室,北京102206

出　　处：《北京农学院学报》2012年第4期73-76,共4页Journal of Beijing University of Agriculture

基　　金：2011第七届北京市教学名师项目;2010年度北京市属高等教育学校人才强教深化计划"学术创新人才"项目(PHR201006124);农产品加工及贮藏工程北京市重点建设学科项目(PXM2009-014207-078172);首都农产品安全产业技术研究院成果转化项目(PXM2012_014207_000019)资助

摘　　要：建立超声辅助分散液相微萃取(USALPME)结合气相色谱火焰光度检测器的新方法,应用于饮用水中的3种有机磷农药(杀螟硫磷、毒死蜱和苯线磷)残留的检测。对可能影响萃取效率的因素,本试验进行优化。结果为:取一只装有5mL水样的离心试管,用移液枪迅速注入30μL氯苯(萃取剂)超声10min,冰浴10min,以3 500r/min离心5min,用微量进样器吸取沉淀相1μL进样分析。在最优条件下,说明3种有机磷农药杀螟硫磷、毒死蜱和苯线磷的检出限为0.41～0.83μg/mL,相对标准偏差为11.94%～16.73%,线性的变化范围(浓度0.5～100μg/mL)在0.995 7～0.999 7之间,此方法检测饮用水中有机磷农药残留结果较满意。A new method, ultrasound assisted liquid phase microextraction （USALPME） combined with Flame Photometry De- tector gas chromatography, was developed to detect three kinds of organophosphorus pesticides, Sumithion, chlorpyrifos, fe- namiphos in potable water. The factors that influenced the extraction were optimized in the experiment. In a centrifugal test tube with 5mL water, the 30μL chlorobenzene （extraction solvent） were injected into the test tube quickly, kept in the ultra- sonic bath for 10 min, ice bath 10 rain, centrifuged at 3500 romin-- 1 for 5 min. 1.0μL of the extractant was injected into GC. At the optimum conditions, the limits of detection for three pesticides ranged from 0.41 to 0. 83μg · L^-1 , the relative stand- ard deviations were between 11.94% and 16.73% , the correlation coefficients varied from 0. 9957 to 0. 9997.

关 键 词：超声辅助 分散液相微萃取 有机磷农药 样品前处理 

分 类 号：O667.7[理学—分析化学]