基于轻质萃取剂的涡旋辅助分散液液微萃取-气相色谱法测定瓶装水中塑化剂
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摘要
以密度比水小的溶剂为萃取剂,建立了涡旋辅助分散液液微萃取-气相色谱检测瓶装水中塑化剂的方法.传统分散液液微萃取技术一般采用密度大于水的有机溶剂为萃取剂.本方法以密度比水小的轻质溶剂正己烷-甲苯(1∶1,体积比)为萃取剂,乙腈为分散剂,涡旋辅助分散,离心后获得富集相,进行气相色谱检测,富集倍数高达171倍,具有良好的线性关系(相关系数为0.998 2~0.999 2)和精密度(3.1%~11.8%),以及较低的方法检出限(1.43~12.05μg/L),加标回收率为81.2%~107.8%.该方法简便,快速,环保,可以用于测定实际水样中塑化剂.
A novel method of low-density solvent-based vortex-assisted dispersive liquid-liquid microextraction(DLLME)was developed for determination of plasticizer in bottled water by gas chromatography-flame ionization detection(GC-FID).Conventional DLLME methods usually employ organic solvents heavier than water as the extraction solvents.On the contrary,in this proposed extraction procedure,a mixture of low-density extraction solvent(toluene and n-hexane with V/V=1∶1)and dispersive solvent(acetonitrile)was injected into the aqueous sample solution to form an emulsion with vortex dispersed mode.The upper layer was collected and analyzed by GC after centrifugation.The enrichment factor was as high as 171.Under the optimized conditions,the proposed method provided a good linearity(R2=0.998 2~0.999 2)and the relative standard deviations(RSDs)were in the range of 3.1%~11.8%.The limits of detection(S/N=3)were in the range of 1.43~12.05μg/L and the recoveries at three spiked levels were in the range of81.2%~107.8%.It is a convenient,speedy,and environmentally benign for the routine analysis of plasticizer in water samples.
A novel method of low-density solvent-based vortex-assisted dispersive liquid-liquid microextraction(DLLME)was developed for determination of plasticizer in bottled water by gas chromatography-flame ionization detection(GC-FID).Conventional DLLME methods usually employ organic solvents heavier than water as the extraction solvents.On the contrary,in this proposed extraction procedure,a mixture of low-density extraction solvent(toluene and n-hexane with V/V=1∶1)and dispersive solvent(acetonitrile)was injected into the aqueous sample solution to form an emulsion with vortex dispersed mode.The upper layer was collected and analyzed by GC after centrifugation.The enrichment factor was as high as 171.Under the optimized conditions,the proposed method provided a good linearity(R2=0.998 2~0.999 2)and the relative standard deviations(RSDs)were in the range of 3.1%~11.8%.The limits of detection(S/N=3)were in the range of 1.43~12.05μg/L and the recoveries at three spiked levels were in the range of81.2%~107.8%.It is a convenient,speedy,and environmentally benign for the routine analysis of plasticizer in water samples.
引文
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[3](EU)No 10/2011On plastic materials and articles intended to come into contact with food[S].
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[13]付博,张吉苹,周璐,等.漂浮液滴固化分散液液微萃取与高效液相色谱联用检测环境水样中的3种烷基苯酚[J].色谱,2017,35(05):533-537.DOI:10.3724/sp.j.1123.2016.12012.FU B,ZHANG J P,ZHOU L,et al.Dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by high performance liquid chromatography for the determination of three alkylphenols in environmental water samples[J].Chinese Journal of Chromatography,2017,35(05):533-537.DOI:10.3724/sp.j.1123.2016.12012.
[14]BAI X Z,ZHANG T,LI H P,et al.Simultaneous dispersive liquid-liquid microextraction based on a low-density solvent and derivatization followed by gas chromatography for the simultaneous determination of chloroanisoles and the precursor 2,4,6-trichlorophenol in water samples[J].Journal of Separation Science,2016,39(11):2146-2155.DOI:10.1002/jssc.201600098.
[2]XU Q,YIN X Y,WANG M.Analysis of phthalate migration from plastic containers to packaged cooking oil and mineral water[J].Journal of Agricultural and Food Chemistry,2010,58(21):11311-11317.DOI:10.1021/jf102821h.
[3](EU)No 10/2011On plastic materials and articles intended to come into contact with food[S].
[4]LV Y K,ZHANG W,GUO M M,et al.Centrifugal microextraction tube-cloud point extraction coupled with gas chromatography for simultaneous determination of six phthalate esters in mineral water[J].Analytical Method,2015,7(2):560-565.DOI:10.1039/c4ay01705f.
[5]RUSSO M V,AVINO P.A critical review on the chromatographic detection of phthalates in different matrices:problems and solutions[C]//MIGUEL OWENS.Phthalates:health effects,detection,and exposure prevention.Hauppauge:New York Nova Science Publishers,Inc,2015:29-60.
[6]SARAJI M,BOROUJENI M K.Recent developments in dispersive liquid-liquid microextraction[J].Analytical&Bioanalytical Chemistry,2014,406(8):2027-2066.DOI:10.1016/j.trac.2011.04.014.
[7]ZGOLA A-GRZES'KOWIAK A,GRZES'KOWIAK T.Dispersive liquid-liquid microextraction[J].TrAC-Trends in Analytical Chemistry,2011,30(9):1382-1399.DOI:org/10.1016/j.trac.2011.04.014.
[8]FARAHANI H,NOROUZI P,DINARVAND R,et al.Development of dispersive liquid-liquid microextraction combined with gas chromatography-mass spectrometry as a simple,rapid and highly sensitive method for the determination of phthalate esters in water samples[J].Journal of Chromatography A,2007,1172(2):105-112.DOI:10.1016/j.chroma.2007.10.001.
[9]REZAEE M,ASSADI Y,MILANI HOSSEINI M R,et al.Determination of organic compounds in water using dispersive liquid-liquid microextraction[J].Journal of Chromatography A,2006,1116(1-2):1-9.DOI:10.1016/j.chroma.2006.03.007.
[10]马燕玲,陈令新,丁养军,等.超声辅助分散液液微萃取-高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂[J].色谱,2013,31(02):155-161.DOI:10.3724/SP.J.1123.2012.09003.MA Y L,CHEN L X,DING Y J,et al.Simultaneous determination of four phthalate esters in water samples using ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography[J].Chinese Journal of Chromatography,2013,31(02):155-161.DOI:10.3724/SP.J.1123.2012.09003.
[11]LEONG M I,HUANG S D.Dispersive liquid-liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron-capture or mass spectrometry detection[J].Journal of Chromatography A,2008,1211(1-2):8-12.DOI.org/10.1016/j.chroma.2008.09.111.
[12]毕欢,郑鑫,伦小文,等.漂浮固化分散液微萃取/气相色谱法测定化妆水中4种增塑剂[J].分析测试学报,2013,32(07):823-828.DOI:10.3969/j.issn.1004-4957.2013.07.007.BI H,ZHENG X,LUN X W,et al.Analysis of phthalate esters in lotion by dispersive liquid-liquid microextraction based on solidification of floating organic droplets combined with gas chromatography[J].Fenxi Ceshi Xuebao(Journal of Instrumental Analysis),2013,32(07):823-828.DOI:10.3969/j.issn.1004-4957.2013.07.007.
[13]付博,张吉苹,周璐,等.漂浮液滴固化分散液液微萃取与高效液相色谱联用检测环境水样中的3种烷基苯酚[J].色谱,2017,35(05):533-537.DOI:10.3724/sp.j.1123.2016.12012.FU B,ZHANG J P,ZHOU L,et al.Dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by high performance liquid chromatography for the determination of three alkylphenols in environmental water samples[J].Chinese Journal of Chromatography,2017,35(05):533-537.DOI:10.3724/sp.j.1123.2016.12012.
[14]BAI X Z,ZHANG T,LI H P,et al.Simultaneous dispersive liquid-liquid microextraction based on a low-density solvent and derivatization followed by gas chromatography for the simultaneous determination of chloroanisoles and the precursor 2,4,6-trichlorophenol in water samples[J].Journal of Separation Science,2016,39(11):2146-2155.DOI:10.1002/jssc.201600098.