固相萃取法处理环境水样中酞酸酯：流速与除水方式的影响  

EXTRACTION OF PHTHALATE ESTERS FROM WATER SAMPLES BY SPE:INFLUENCE OF FLOW RATE AND DEHYDRATION PROCEDURE

作　　者：陈永山[1,2] 骆永明[1,2] 章海波[1] 宋静[1] 黄玉娟[1] 

机构地区：[1]中国科学院土壤环境与污染修复重点实验室(南京土壤研究所),土壤与环境生物修复中心,南京210008 [2]中国科学院研究生院,北京100049

出　　处：《环境化学》2010年第5期954-959,共6页Environmental Chemistry

基　　金：国家水体污染控制与治理科技重大专项课题(2008ZX07101-006-05);中国科学院“优秀博士学位论文、院长奖获得者科研启动专项资金”资助

摘　　要：利用固相萃取结合气相色谱-质谱联用分析探讨了不同过柱流速、过柱后除水方式等对水样加标回收率的影响,同时还比较了3种C18填料的商品柱对分析方法的空白和回收率影响.结果表明,采用500mg/3ml的常规小柱足以分析水环境的酞酸酯含量.水样过柱流速最好保持在3ml.min-1左右,过完水样后不可抽干小柱,用6m.lmin-1氮气吹小柱20min后,洗脱液再过无水硫酸钠,可获得较为理想的回收率.萃取柱的材质对分析方法空白有一定影响,玻璃小柱要比塑料小柱的空白低,但从可操作性和满足回收率的要求角度出发,小容积的塑料小柱基本能满足酞酸酯的痕量分析要求.Contamination of phthalate esters（PAEs） in aquatic environment has been of wide concern owing to the endocrine disruption effect of these compounds.Solid phase extraction（SPE） combined with gas chromatograph-mass spectrometer（GC-MS） were performed to study the influence of flow rate and dehydration procedure on the recovery of the added standard.In addition three types of tubes filled with C18 frequently used among the laboratories were evaluated.The results indicated that small plastic tubes（500mg/3ml） were capable of enriching the PAEs from water samples effectively.Water flow rate passing through the cartridge should be below 3ml·min^-1,and the tube should be blew gently by with nitrogen gas for 20min at the speed of 6ml·min^-1 to remove water after enrichment.Then the eluate washed from the tube was passed through a glass column containing anhydrous sodium to dehydrate completely.Materials of the tube have an impact on the procedure blank.Lower procedure blanks were observed with glass tubes than with plastic tubes.However,plastic tube with small volumes are still recommended to be applied in the SPE procedure in view of them convenience as well as meeting the requirement of the recovery.

关 键 词：酞酸酯 固相萃取 回收率 水环境 

分 类 号：X832[环境科学与工程—环境工程]