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1、20143,】色譜VO1.32No.3March2014ChineseJournalofChromatography256~262研究論文DOI:1().3724/SP.J.1l23.20l3,l】004摘要:建●:r分敞液}f芷微咎取(DLLME)一反十H液液微萆取(RP—LLME)寸1一膠求動(dòng)色i集模,j¨,:l:酒叫I』l酚(PCP)、2,4,6一二二氯『lij}(TCP)和2,4-二氯酚(DCP)3種氯盼的測(cè)定。實(shí)驗(yàn)芎察r兩步微畢收的取參數(shù)對(duì)氯酚畢取的影響和樣出分離富集的電泳條件最萃取條件DLLME為:3.5mLI:
2、灑(pH3.0,120g/LNaCI),300LJIL二烷(蘋取刷);RP-LLME為:25L0.16mol/LNaOH(芊取劑).電泳條什:25mmol/LNailPO,100mmol/L卜二烷旗硫酸鈉(SDS),30%(v/v)乙腈,pH2.3;分離電一l5kV;樣品質(zhì)為80mmol/LNailPO;力進(jìn)樣20sx20.67kPa(3psi)PCP和TCP的線性范為0.5~l00g/L(r≥0.99l0),DCP的線一范剛為1.5~80g/L(r=0.9851)3種分析物的榆出限(Ⅳ=3)為0.035~0.Il4g/L,
3、杯叫收半為75.2%~l04.7%,相對(duì)準(zhǔn)偏差≤6.17%該方法謝集倍數(shù)島、靈敏度商、承脫好、分析速度怏,_I『為小樣5f·質(zhì)rf『j良fIt氯附污染物及些弱酸有機(jī)污染物測(cè)定提供參學(xué)、關(guān)鍵詞:分敞液液微?。环词甀I液液微畢??;捫集;膠求}乜動(dòng)色譜;氯酚;紅f『If中圖分類號(hào):O658文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):l000—87l3(20l4)03—0256—07Abstract:Amethodofdispersiveliquid—liquidmicr0extraction(DLLME)andreversedphaseliquid—
4、liquidmicroextraction(RP—LLME)procedurescoupledwithsweeping—micellarelectroki—neticchromatography(sweeping—MEKC)wasestablishedtoextractanddeterminethethreechlorophenols(CPs)includingpentachlor0phenol(PCP),2,4,6-tnchlorophenol(TCP)and2,4-dichlorophenol(DCP)inredwine
5、.Theinfluencesoftheparametersoftwoextractionstepsandtheelectr0phoresisconditionswereinvestigated.Theoptimumextractionconditionswereasfollows:forDLLME,3.5mLredwinesample(pH3.0,l20g/LNaC1),300uLhexane(extractionsolvent),extractionfor3min,centrifugationfor3rainat5000r
6、/rain;forRP—LLME,25L0.16mol/LNaOHsolution,extractionfor2min,centrifugationfor2rainat5000r/min.Theoptimumrunningbuffer(pH2.3)wasanaqueoussolutioncontaining25mmol/LNail,PO,100mmol/Lsodiumdodecylsulfate(SDS)and30%(v/v)acetonitrile.Theopti—mumon—linec0ncentrationcondit
7、ionswereasfollows:samplematrix,80mmol/LNailPOJ;hydrodynamicinjectionof20sat20.67kPa(3psi).Undertheoptimumconditions,theexcel—lentlinearitywasobtainedovertherangeof0.5—100jxg/L(r≥0.99l0)forPCPandTCP,and1.5—80g/L(r≥0.9851)forDCP.Thelimitsofdetection(./N=3)wereinthera
8、ngeof:#通訊聯(lián)系人.E—mail:shliu8l50、I26corn.基金項(xiàng)目:北農(nóng)林利技人學(xué),j1進(jìn)人’々項(xiàng)肇金順lj(ZIl1021005)收稿日期:20l3一lI一04第3期孫建芝,等:分散液液微萃取一反相液液微萃取一掃集一膠束電動(dòng)色譜法測(cè)定紅酒中的3種氯酚類物質(zhì)‘257。0.