色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
6期
623-628
,共6页
王晓燕%亓伟梅%赵先恩%吕涛%王西亚%郑龙芳%闫业浩%尤进茂
王曉燕%亓偉梅%趙先恩%呂濤%王西亞%鄭龍芳%閆業浩%尤進茂
왕효연%기위매%조선은%려도%왕서아%정룡방%염업호%우진무
分散液液微萃取%衍生化%高效液相色谱%荧光检测%酚类化合物%内分泌干扰物%环境水样
分散液液微萃取%衍生化%高效液相色譜%熒光檢測%酚類化閤物%內分泌榦擾物%環境水樣
분산액액미췌취%연생화%고효액상색보%형광검측%분류화합물%내분비간우물%배경수양
dispersive liquid-liquid microextraction( DLLME)%derivatization%high perform-ance liquid chromatography( HPLC)%fluorescence detection( FLD)%phenols%endocrine dis-ruptors%environmental water samples
为实现小体积环境水样中酚类化合物的准确、快速、高灵敏测定,通过分散液液微萃取( DLLME)和荧光衍生化的结合,建立了高效液相色谱-荧光检测(HPLC-FLD)双酚 A、壬基酚、辛基酚和对特辛基酚的分析方法。考察并优化了 DLLME 和衍生化条件,结果表明,最优的 DLLME 条件为萃取剂氯仿用量70μL,分散剂乙腈用量400μL,漩涡振荡3 min,高速离心2 min。以2-[2-(7H-二苯并[a,g]咔唑-乙氧基)]-乙基氯甲酸酯(DBCEC-Cl)为柱前衍生试剂,在 pH 10.5的 Na2 CO3-NaHCO 3缓冲液/乙腈溶液、50℃下衍生反应3 min 得到稳定的衍生产物,于10 min 内实现了4种酚衍生物的分离。方法的检出限为0.9~1.6 ng / L,定量限为3.8~7.1 ng / L,具有良好的线性、精密度和回收率,与以往报道的方法相比具有一定的优势和实用性,可用于造纸厂废水、湖水、生活废水、自来水中4种酚类内分泌干扰物的测定。
為實現小體積環境水樣中酚類化閤物的準確、快速、高靈敏測定,通過分散液液微萃取( DLLME)和熒光衍生化的結閤,建立瞭高效液相色譜-熒光檢測(HPLC-FLD)雙酚 A、壬基酚、辛基酚和對特辛基酚的分析方法。攷察併優化瞭 DLLME 和衍生化條件,結果錶明,最優的 DLLME 條件為萃取劑氯倣用量70μL,分散劑乙腈用量400μL,漩渦振盪3 min,高速離心2 min。以2-[2-(7H-二苯併[a,g]咔唑-乙氧基)]-乙基氯甲痠酯(DBCEC-Cl)為柱前衍生試劑,在 pH 10.5的 Na2 CO3-NaHCO 3緩遲液/乙腈溶液、50℃下衍生反應3 min 得到穩定的衍生產物,于10 min 內實現瞭4種酚衍生物的分離。方法的檢齣限為0.9~1.6 ng / L,定量限為3.8~7.1 ng / L,具有良好的線性、精密度和迴收率,與以往報道的方法相比具有一定的優勢和實用性,可用于造紙廠廢水、湖水、生活廢水、自來水中4種酚類內分泌榦擾物的測定。
위실현소체적배경수양중분류화합물적준학、쾌속、고령민측정,통과분산액액미췌취( DLLME)화형광연생화적결합,건립료고효액상색보-형광검측(HPLC-FLD)쌍분 A、임기분、신기분화대특신기분적분석방법。고찰병우화료 DLLME 화연생화조건,결과표명,최우적 DLLME 조건위췌취제록방용량70μL,분산제을정용량400μL,선와진탕3 min,고속리심2 min。이2-[2-(7H-이분병[a,g]잡서-을양기)]-을기록갑산지(DBCEC-Cl)위주전연생시제,재 pH 10.5적 Na2 CO3-NaHCO 3완충액/을정용액、50℃하연생반응3 min 득도은정적연생산물,우10 min 내실현료4충분연생물적분리。방법적검출한위0.9~1.6 ng / L,정량한위3.8~7.1 ng / L,구유량호적선성、정밀도화회수솔,여이왕보도적방법상비구유일정적우세화실용성,가용우조지엄폐수、호수、생활폐수、자래수중4충분류내분비간우물적측정。
To achieve accurate,fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples,a method of dispersive liquid-liquid microextrac-tion(DLLME)coupled with fluorescent derivatization was developed for the determination of bisphenol A,nonylphenol,octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection( HPLC-FLD). The DLLME and derivatization conditions were investigated,and the optimized DLLME conditions for small volume of environmental water samples(pH 4. 0)at room temperature were as follows:70 μL chloroform as extraction solvent,400 μL acetonitrile as dispersing solvent,vortex mixing for 3 min,and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo[ a,g]carbazol-7-yl)-ethoxy]ethyl chloroformate( DBCEC-Cl)as precolumn derivatization reagent,the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10. 5 Na 2 CO 3-NaHCO 3 buffer / acetonitrile at 50 ℃ for 3 min,and then separated within 10 min by HPLC-FLD. The lim-its of detection( LODs)were in the range of 0. 9 - 1. 6 ng / L,and the limits of quantification (LOQs)were in the range of 3. 8-7. 1 ng / L. This method had perfect linearity,precision and recovery results,and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill,lake water,domestic wastewater,tap water,etc.