化学试剂
化學試劑
화학시제
CHEMICAL REAGENTS
2010年
3期
239-242
,共4页
廖艳%余煜棉%赖子尼%齐素芳
廖豔%餘煜棉%賴子尼%齊素芳
료염%여욱면%뢰자니%제소방
优化%计算机拟和技术%固相萃取%气相色谱法
優化%計算機擬和技術%固相萃取%氣相色譜法
우화%계산궤의화기술%고상췌취%기상색보법
optimization%CRT technology%solid phase extraction%GC
利用固相萃取技术富集了水中6种邻苯二甲酸酯类:邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)、邻苯二甲酸丁基苄基酯(BBP).借助均匀设计法及计算机回归建模优化技术对6种邻苯二甲酸酯类的固相萃取条件进行了设计与优化,得到最佳固相萃取条件为:洗脱剂配比(正己烷与丙酮的体积比)30∶1,洗脱体积2 mL,洗脱速率为4 mL/min,上样速率8 mL/min.富集后的样品用带电子捕获器的毛细管气相色谱检测,方法的线性范围为1~1 000 μg/L(DMP、DEP、DOP),0.2~100 μg/L(DBP、DEHP),0.1~100 μg/L(BBP);线性回归方程的相关系数为0.997 0~1.000,检测限为0.01~0.4 μg/L,方法回收率为69.0%~117.0%,相对标准偏差为2.2%~9.5%.
利用固相萃取技術富集瞭水中6種鄰苯二甲痠酯類:鄰苯二甲痠二(2-乙基己基)酯(DEHP)、鄰苯二甲痠二甲酯(DMP)、鄰苯二甲痠二乙酯(DEP)、鄰苯二甲痠二丁酯(DBP)、鄰苯二甲痠二辛酯(DOP)、鄰苯二甲痠丁基芐基酯(BBP).藉助均勻設計法及計算機迴歸建模優化技術對6種鄰苯二甲痠酯類的固相萃取條件進行瞭設計與優化,得到最佳固相萃取條件為:洗脫劑配比(正己烷與丙酮的體積比)30∶1,洗脫體積2 mL,洗脫速率為4 mL/min,上樣速率8 mL/min.富集後的樣品用帶電子捕穫器的毛細管氣相色譜檢測,方法的線性範圍為1~1 000 μg/L(DMP、DEP、DOP),0.2~100 μg/L(DBP、DEHP),0.1~100 μg/L(BBP);線性迴歸方程的相關繫數為0.997 0~1.000,檢測限為0.01~0.4 μg/L,方法迴收率為69.0%~117.0%,相對標準偏差為2.2%~9.5%.
이용고상췌취기술부집료수중6충린분이갑산지류:린분이갑산이(2-을기기기)지(DEHP)、린분이갑산이갑지(DMP)、린분이갑산이을지(DEP)、린분이갑산이정지(DBP)、린분이갑산이신지(DOP)、린분이갑산정기변기지(BBP).차조균균설계법급계산궤회귀건모우화기술대6충린분이갑산지류적고상췌취조건진행료설계여우화,득도최가고상췌취조건위:세탈제배비(정기완여병동적체적비)30∶1,세탈체적2 mL,세탈속솔위4 mL/min,상양속솔8 mL/min.부집후적양품용대전자포획기적모세관기상색보검측,방법적선성범위위1~1 000 μg/L(DMP、DEP、DOP),0.2~100 μg/L(DBP、DEHP),0.1~100 μg/L(BBP);선성회귀방정적상관계수위0.997 0~1.000,검측한위0.01~0.4 μg/L,방법회수솔위69.0%~117.0%,상대표준편차위2.2%~9.5%.
One of the environmentally-friendly sample preconcentration technologies the solid phase extraction(SPE) coupled with GC-ECD was employed in the trace analysis of phthalate esters,namely dimethyl phthalate(DMP),diethyl phthalate(DEP),di-n-butyl phthalate(DBP),di-2-ethylhexyl phthalate(DEHP),dioctyl phthalate(DOP),and butyl benzyl phthalate(BBP).Several SPE conditions were optimized by means of homogeneous design and the related mathematical model obtained by computer regressive analysis.The optimal conditions of SPE obtained were volume,4 mL/min for the elution flow rate,and 8 mL/min for the sampling flow rate.The linear response of the proposed method was in the range of 1~1 000 μg/L for DMP,DEP,and DOP;0.2~100 μg/L for DBP and DEHP;and 0.1~100 μg/L for BBP.The correlation coefficient of the regression equation was in the range of 0.997 0~1.000.The detection limits of the method were 0.01~0.4 μg/L.The recovery efficiencies were in the range of 69.0%~117.0% and the RSDs were in the range of 2.2%~9.5%.