Matrix solid-phase dispersion MSPD 6 Solid phase extraction SPE 8. Accelerated solvent extraction ASE 3 9 Solid phase microextraction SPME 10

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1 FENXI HUAXUE Chinese Journal of Analytical Chemistry 1 67 ~ 71 * ph ~ 200 μg /L LOD S /N = ~ μg /L LOQ S /N = ~ μg /L % ~ % A 1 Alkylphenols Aps 1 A Bisphenol A BPA A BPA OP NP N- 2 nonylphenol NP octyphenol OP BPA BPA OP NP BPA OP NP - Liquid-liquid extraction LLE 7 Matrix solid-phase dispersion MSPD 6 Solid phase extraction SPE 8 Accelerated solvent extraction ASE 3 9 Solid phase microextraction SPME 10 Hollow fiber membrane extraction HFME 10 LLE MSPD SPE ASE SPME HFME Stir bar sorptive extraction SBSE SPME Sandra 1999 Gerstel SBSE Polydimethylsiloxane PDMS SPME 25 ~ 250 ml 11 SBSE 13 SPME SBSE PDMS PDMS Stir bar for sorption extraction based on monolithic material SBSEM 16 ~ 19 SBSE SBSEM No No. 2006F3117 * hxj@ xmu. edu. cn

2 68 38 N- - BPA OP NP ph HPLC- DAD LC-20AB CBA-20A SPD-M20A DAD Shimadzu Kyoto 7725i Rheodyne 20 μl Commercial stir bars SBSEC PDMS 20 mm 1. 0 mm Twister Gerstel Müllheim a /d Ruhr Germany SBSEM 30 mm 6 mm N mm 12 BPA 99% TCI OP 99. 7% NP 99% Augsburg Tedia Milli-Q Millipore mg 25 ml 100 mg /L μm 2. 3 Kromasil LC mm 4. 5 mm i. d. 5 μm A - B 1. 0 ml /min 276 nm 20 μl 0 ~ 5 min 60% B 5 ~ 10 min 60% ~ 100% B 10 ~ 20 min 100% B 20 ~ 25 min 100% ~ 60% B ml 250 ml 200 r /min 3. 0 ml 0. 5 ml h 1. 5 h 1. 5 h BPA OP NP 1. 5 h 1. 5 h 1. 0 h SBSEM 1. 0 h ~ 20 1 SBSEM Fig. 1 Effect of extraction time on extraction efficiency 1. A Bisphenol A BPA 2. Nonyphenol NP NaCl 3. Octyphenol OP g /ml 2a NaCl 0 ~ g /ml SBSEM

3 1 69 NaCl NaCl 16 ~ NaCl 19 2a BPA NP NaCl g /ml OP NaCl g /ml g /ml NaCl g /ml ph ph b BPA ph = 7. 0 OP ph = 4. 0 ph = 7. 0 NP ph = 3. 0 ph = ph ph Fig. 2 a ph b Effect of ionic strength a and ph value b on extraction efficiency 1. A BPA 2. OP 3. NP LOD S /N = ~ μg /L LOQ S /N = ~ μg /L RSD < 10% 1 3 Table 1 Linear dynamic range correlation coefficients LODs and LOQs inter-day and intra-day precisions achieved for the three phenols * Linear Range μg /L r LOD μg /L LOQ μg /L Intra-day RSD Inter-day RSD % n = 3 % n = 3 BPA 1. 0 ~ OP 3. 0 ~ NP 3. 0 ~ * Spiked level includes μg /L 3. 3 SBSEC μg /L 2 SBSEC SBSEM PDMS 3 SBSEC SBSEM 2 Table 2 Extractive efficiency of stir bar for sorption extraction based on monolithic material SBSEM and stir bar sorptive extraction SBSE and commercial stir bar for sorption extraction material SBSEC for analytes BPA Peak area OP Peak area NP Peak area SBSEC SBSEM

4 SBSEM SBSEM HPLC-DAD μg /L BPA NP LOQ μg /L BPA 3 OP μg /L % ~ 99. 4% RSD Fig. 3 HPLC chromatograms of three phenols a 100 μg /L Spiked wastewater sample 3. 0% ~ 9. 9% 100 μg /L 3 with each phenolic compounds at 100 μg /L and treated with SB % ~ % SEM b Wastewater sample treated RSD 2. 0% ~ 9. 8% with SBSEM c Direct injection of wastewater sample 1 A BPA 2 OP 3 NP RSD < 10% 3 Table 3 Results of determination and recoveries of real water samples spiked with three target analytes Water sample Wastewater inlet Wastewater outlet Seawater * ND Not detected Added μg /L Found μg /L BPA OP NP Recovery % n = 3 BPA OP NP ND ND ± ± ± ± ± ± ND ND ± ± ± ± ± ± ND ND ± ± ± ± ± ± 8. 8 References 1 REN Ren CHEN Ming WU Shao-Hua ZHANG Shu-Fen WANG Gui-Hua. J. Beijing Univ. Tech ~ 24 2 Renner R. Envrion Sci. Technol ~ SHAO Bing HAN Hao LI Dong-Mei ZHAO Rong MENG Juan MA Ya-Lu. Chinese Journal of Chromatography ~ SHAO Bing GAO Ying-Xin HAN Hao ZHAO Rong MENG Juan WU Guo- Hua. Environ. Chem ~ Ballesteros O Zafra A Naval on A V lchez J L. J. Chromatogr. A ~ L Gang WANG Li-Bing LIU Jun ZHANG Shu-Fen. Chinese J. Anal. Lab ~ 80 7 XIAO Shang-You WANG Jie-Feng XIA Zhi-Ning MU Xiao-Jing. Chinese J. Anal. Chem ~ 1196

5 ZHANG Hong MAO Jong SUN Cheng-Jun WU De-Sheng MAO Li-Sha Chinese Journal of Chromatography ~ WANG Jing PAN He-Fang WEN Ying LIU Jin-Song. Environmental Monitoring in China ~ Basheer C Parthiban A Jayaraman A Lee H K Valiyaveettil S. J. Chromatogr. A /2 274 ~ Baltussen E Sandra P David F Cramers C. J. Microcol. Sep ~ David F Sandra P. J. Chromatogr. A ~ Bicchia C Cordero C Liberto E Rubiolo P Sgorbini B Sandra P. J. Chromatogr. A ~ Demyttenaere J C R Morina R M De Kimper N Sandra P. J. Chromatogr. A ~ YU Chun-He HU Bin JIANG Zu-Cheng. Chinese J. Anal. Chem ~ Huang X J Qiu N N Yuan D X. J. Chromatogr. A ~ Huang X J Qiu N N Yuan D X. J. Chromatogr. A ~ Huang X J Lin J B Yuan D X Hu R Z. J. Chromatogr. A ~ Huang X J Yuan D X. J. Chromatogr. A ~ 157 Determination of Alkylphenol in Water Samples by Stir Bar Sorptive Extraction Based on Poly vinylimidazole-divinylbenzene Monolithic Material and Liquid Chromatographic Analysis LIN Fu-Hua QIU Ning-Ning HUANG Xiao-Jia * YUAN Dong-Xing State Key Laboratory of Marine Environmental Science Environmental Science Research Center Xiamen University Xiamen Abstract A method for the determination of bisphenol A octyphenol nonylphenol in water samples was developed using stir bar sorptive extraction SBSE based on poly vinylimidazole-divinylbenzene monolithic material SBSEM combined with high performance liquid chromatography with diode array detection. To achieve the optimum extraction performance several main extraction parameters including extraction and desorption time ph value and contents of inorganic salt in the sample matrix were investigated. Under the optimized experimental conditions the method showed good linearity and repeatability low detection limits S /N = 3 and quantification limits S /N = 10 of the proposed method for the target compounds were achieved within the range of and μg /L respectively. The extraction performance of SBSEM to the target compounds was also compared with commercial SBSE which used polydimethylsiloxane as coating. The proposed method was successfully applied to the determination of the target compounds in water samples. The recoveries of spiked target compounds in real samples ranged from 37. 8% %. The results indicated that the developed method possessed advantages such as sensitivity simplicity low cost and high feasibility. Keywords Stir bar sorptive extraction Monolithic material High performance liquid chromatography /diode array detector Bisphenol A Octyphenol Nonylphenol Received 15 July 2009 accepted 26 September 2009

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