SFO-DLLME 12 DLLME DLLME SFO-DLLME. 1 L NaCl 1 mol /L H 3 PO 4

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1 FENXI UAXUE Chinese Journal of Analytical Chemistry ~ 1404 DOI /P. J * FO-DLLME μl 300 μl 1. 2 g NaCl 1 mol /L 3 PO μl 8. 0 ml 3 min ~ 6. 0 mg /L 20 ~ 38 μg /L % ~ % 3. 5% ~ 4. 6% Lai DLLME 8 9 ~ 11 - FO-DLLME 12 DLLME DLLME FO-DLLME CP DCP DCP Agilent Agilent ACRO 1. 0 g /L 1. 0 ml ml ml L 4 1- V V = 2 1 NaCl 1 mol /L 3 PO 4 TEDIA No. Q * dzqyx@ yahoo. cn

10 - - 1401 2. 2 Tc-C 18 150 mm 4. 6 mm 5 μm Agilent V V = 70 30 1. 0 ml /min 245 nm 30 20 μl 2. 3 10 ml 8. 0 ml 1.

2 Tc-C mm 4. 6 mm 5 μm Agilent V V = ml /min 245 nm μl ml 8. 0 ml 1. 2 g NaCl 200 μl 1 mol /L 3 PO μl 1a 200 μl V /V 3 min 1b 3000 r /min 2 min 1c 0 3 min 1d 50 μl 20 μl DLLME mp mp mp 38 Fig. 1 Photograph of different steps in dispersive mp 18 liquid-liquid microextraction base on solidification 1- of floating organic FO-DLLME 1- a. Water sample b. 1- Emulsion of water sample after 1- injection of mixture of extraction and disperser solvent V /V 2 c. After centrifuging floating extraction solvent droplet d. olidification of floating organic drop 200 μl 200 μl 200 μl μl 300 μl NaCl 1. 2 g NaCl 1. 2 g NaCl 15 1 mol /L 3 PO 4 3 PO μl

3 Fig. 2 Optimization of extractant volume 1. 0 mg /L 2-chlorophenol 2-CP 1. 0 mg /L 2-6-dichlorophenol 2- CP 2 6-DCP 0. 4 mg /L 2 4-DCP. 300 μl methanol 1. 2 g NaCl 200 μl 1 mol /L 3 PO ml Mixed standard solution. 3 Fig. 3 Optimization of dispersive solvent 2 Experimental conditions are same as in Fig. 2 3 PO 4 p μl 1 mol /L 3 PO 4 p = ml 8. 0 ml 8. 0 ml 3 min 3 min 3. 5 LOD /N = mg /L Table 1 Linear equation limit of detection RD and enrichment factor for three kinds of chlorophenols RD % Linear range Analyte Linear equation r 2 Detection limit Enrichment mg /L factor Intra-day Inter-day 2-CP y = c ~ DCP y = c ~ DCP y = c ~ LPME LPME 2-CP 2 6-DCP -LPME 2 - Table 2 Comparison of FO-DLLME method and -LPME method Analyte Extraction time min Detection limit Linear range RD Intra-day RD % Inter-day RD % 2-CP ~ ~ DCP ~ ~ DCP ~ ~ eadspace liquid-phase microextraction -LPME - Dispersive liquid-liquid microextraction based on solidification of floating organic FO-DLLME

4 μm % ~ % 4 4 Fig. 4 Chromatograms of sample determination A. Blank water sample B C. piked water sample B mg /L C 0. 5 mg /L 1. 2-CP DCP DCP R olvent peak 10 min 3 Table 3 Analytical results of samples ample Tap water Water of anjiang river Added mg /L ND. Not detected 2-CP Found mg /L 2 6-DCP 2 4-DCP 2-CP Recovery % n = DCP 2 4-DCP ND ND ND ND References 1 Tsuji N irooka T Nagase irata K Miyamoto K. Biotechnol. Lett ~ Feng Q Z Zhao L X Yan W Ji F. Anal. Bioanal. Chem ~ Lai B W Liu B M Malik P K Wu F. Anal. Chim. Acta ~ 66 4 CAI Min WANG Wei XING Jun FENG Yu-Qi WU Cai-Ying. Chinese J. Anal. Chem ~ 94 5 Tor A Cengeloglu Y Aydin M E Wichmann Bahadir M. Fresenius Environmental Bulletin B 1329 ~ Portillo M Prohibas N alvado V imonet B M. J. Chromatogr. A ~ 34 7 ZANG Xiao-uan WU Qiu-ua ZANG Mei-Yue XI Guo-ong WANG Zhi. Chinese J. Anal. Chem ~ Rezaee M Assadi Y Milani M R Aghaee E Ahmadi F Berijani. J. Chromatogr. A ~ 9 9 ZANG Yan-Jie BAI Xiao-ong LI Li-ua WANG Quan-De. Chinese J. Anal. Chem ~ DING Zong-Qing LIU Guang-Dong. Chinese J. Anal. Chem ~ Chiang J uang D. Talanta ~ Leong M I uang D. J. Chromatogr. A ~ Wei G Li Y Y Wang X D. J. ep. ci ~ Basheer C Lee K Obbard J P. J. Chromatogr. A ~ Zhao L M Lee K. J. Chromatogr. A ~ 105

5 Buchholz K D Pawliszyn J. Anal. Chem ~ Xu Liao Y Yao J R. J. Chromatogr. A ~ 8 Dispersive Liquid-Liquid Microextraction Based on olidification of Floating Organic Drop Combined with igh Performance Liquid Chromatography for Determination of Chlorophenols in Aqueous amples DING Zong-Qing * 1 ZANG Qiong-Yao 2 1 Department of Chemistry Yunyang Teachers College Danjiangkou Department of Comment Medicinal Chemistry ubei Medical College hiyan Abstract Using the method of dispersive liquid liquid microextraction based on solidification of floating organic DLLME-FO combined with PLC three kinds of chlorophenols in aqueous samples were determined. The DLLME method with 1-dodecanol whose density was less than water and freezing point was 24 utilized as extractant and methanol as dispersive solvent was applied to analyze water samples. After the mixture was centrifugaled the floated extractant that was solidified in ice bath was easily removed from water phase. When the solidified extractant droplet was redissolved it was injected into the PLC for analysis. The optimal experiment conditions were as follows extractant solvent 200 μl dispersive solvent 300 μl NaCl 1. 2 g 1 mol /L 3 PO μl sample volume 8. 0 ml extraction time 3 min. The calibration curve was linear in the range of mg /L of the three kinds of chlorophenols and the detection limits were μg /L. This method has been applied to the determination of real water samples the recovery of standard additions were from % to % and the inter-day RDs were between 3. 5% and 4. 6%. The method extended the range of choosing the extractant in DLLME it was proven to be simple rapid accurate and environment friendly. Keywords Dispersive liquid liquid microextraction based on solidification of floating organic igh performance liquid chromatography Chlorophenol 1-Dodecanol eparation and enrichment Received 23 March 2010 accepted 22 April 2010 櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞櫞 " "

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