38 200 4 FENXI HUAXUE Chinese Journal of Analytical Chemistry 4 503 ~ 507 DOI 0. 3724 /SP. J. 096. 200. 00503 6 - A * 2 2 * 2 20009 2 20096 6 - A ph 6 0 ml ph 8. 0 3 ml /min. 5 mg 6 300 μl A 6 0. 20 ~ 20. 0 μg /L 0. 5 μg /L 4. 5% n = 6 6 A. 0 μg /L 95. 0% A 0. 30 μg /L 6 6 A A Biphenol A BPA BPA 2 BPA 3 4 LLE 5 SPE 3 6 7-8 9 0 Electrospinning Kang 2 Packed-fiber solid-phase extraction PFSPE ml 6 6 6 2009-07-6 2009-09- No. 50533030 No. BK2006509 * E-mail q_xu@ 63. com Qian Xu gu@ seu. edu. cn Zhongze Gu
504 38 - BPA BPA 2 2. LC-0AD SPD0-Avp TL-9900 78- phs-2c DW- P403-AC Hitachi S-3000N Tedia 6 M w. 6 0 4 BPA Sigma. 0 g /L BPA 2. 0% V /V 6 2. 2 ODS 250 mm 4. 6 mm 5μm Dikma - 60 40 V /V 0. 8 ml /min 230 nm 20 μl 30 2. 3 6-6 4 V /V 2 h 30% w /V 6 0. 5 mm 0. 5 ml /h 20 cm 5 kv Taylor 5 ~ 0 h 00 ~ 300 μm Hitachi S-3000N 3A 00 ~ 300 nm 2. 4. 8 cm 2 - - -0. 2 ml 6 l0 ml 3 ml /min 300 μl N 2 50 μl 2 Fig. Schematic diagram of electrospinning Fig. 2 Solid-membrane extraction device 3 3. 3.. 6 0. 5 ~ 3. 0 mg A 0. 5 mg. 5 mg
4 6 - A 505. 5 mg 6 RSD = 3. 2% 3.. 2 ph ph BPA 6 ph BPA 6 BPA 6 ph 3 3B ph 4 ~ BPA 4 ph = 8 3 6 ph 8 A ph 3 B 3.. 3 Fig. 3 Scanning electron microscope images of nylon 6 nanofibrous membrane at ph 8 A at ph 3 B ~ 5 ml /min ml /min 3 ml /min 90. 7% ± 2. % n = 3 3 ml /min 3.. 4 0. ~ 0. 5 ml 20% 50% 80% - 0. 3 ml BPA 3.. 5 4 ph Fig. 4 Effect of ph on the recovery of biphenol A BPA BPA 6 0 ml 94. 6% ± 3. 0% n = 3 3. 2 0. 20 ~ 20. 00 μg /L r = 0. 9998 S /N = 3 0. 5 μg / L n = 6 3. % 4. 4%. 0 μg /L n = 6 95. 0% ± 2. 8% Table Results of determination and recoveries of real water samples spiked with BPA 3. 3 Found Added level RSD Sample Recovery % n = 3 μg /L μg /L 6 ND. 0 93. 3 2. 5 BPA 6 2 0. 2. 0 94. 8 2. 3 ND. 0 93. 8 2. 3 3 BPA 4 0. 20. 0 95. 2. 4 0. 2 0. 20 0. 30 μg /L 5 5 0. 30. 0 94. 2 2. 7 6 ND. 0 94. 0 3. 0 3. 4 ND Not detected. BPA 3 ~ 5
506 38 2 6 5 Fig. 5 a. 0 μg /L b c Chromatograms of standard solution a sample spiked with. 0 μg /L b and water sample c for BPA 2 Table 2 Comparison with other s in literatures Quality of Organic solvent RSD LOD μg /L % Recovery % sorbent mg ml Sorbents OASIS- HLB 200 2. 0 4. 8 96. 5 3 C 8. 5 500. 0 2 0. 5. 2 4. 43 3. 7 94. 9 95. 8 4 Bamboo- charcoal 0 0. 7 3. 0 90. 7 5 References Kavlock R J. Chemosphere 999 39 8 227 ~ 236 2 HU Xiang-Wei ZHANG Wen-De LIU Yan-Qiao. Chinese J. Foods Science 2006 27 4 264 ~ 266 3 CHEN Su-Qing LIANG Hua-Ding HUANG Wei-Ya HAN De-Man WANG Xi- Mei. Chinese J. Anal. Chem. 2008 36 7 959 ~ 963 4 MIAO Jia-Zheng XUE Ming ZHANG Hong. Chinese J. Aanl. Chem. 2009 37 6 9 ~ 94 5 ZHOU Jian-Ke ZHANG Qian-Li HAN Kang ZHANG Li ZHAO Fei-Bao. Chinese Journal of Science and Technology of Food Industry 2007 28 2 233 ~ 234 6 Cao X L Corriveau J Popovic S Clement G Beraldin F Dufresne G. Agric. Food Chem. 2009 57 2 5345 ~ 535 7 Grumetto L Montesano D Seccia S Alriizio S Barbato F. Agric. Food Chem. 2008 56 22 0633 ~ 0637 8 McDowall R D. J. Chromatogr. B 989 492 6 3 ~ 58 9 Lu P Ding B. Recent Pat Nanotechnol 2008 2 3 69 ~ 82 0 Gibson P Schreuder-Gibson H Rivin D. Colloids and Surface A-Physicochemical and Engineering Aspects 2nd Ed. Princeton Characterization of Porous Materials 200 87 469 ~ 48 Kang X J Pan C Xu Q Yao Y F Wang Y Qi D J Gu Z Z. Anal. Chim. Acta 2007 587 75 ~ 8 2 Qi D J Kang X J Chen L Q Zhang Y Y Wei H M Gu Z Z. Anal. Bioanal. Chem. 2008 390 3 929 ~ 938 3 HAN Hao SHAO Bing MA Ya-Lu WU Guo-Hua ZHAO Ying. Chinese Journal of Chromatography 2005 23 4 362 ~ 365 4 WANG Xiao-Dong ZHAO Xin-Hua ZHANG Xin-Bo LI Hong-Xia XUE Yan. Chinese Journal of Analysis Laboratory 2006 25 9 27 ~ 29 5 Zhao R S Wang X Yuan J P Zhang L L. Microchim. Acta 2009 65 443 ~ 447
4 6 - A 507 Determination of Bisphenol A in Plastic Bottled Drinking Water by High Performance Liquid Chromatography with Solidmembrane Extraction Based on Electrospun Nylon 6 Nanofibrous Membrane WU Shu-Yan XU Qian * 2 CHEN Tian-Shu WANG Min YIN Xue-Yan ZHANG Ni-Ping SHEN Yan-Yan WEN Zuo-Yang 2 GU Zhong-Ze * 2 School of Public Health Southeast University Nanjing 20009 2 State Key Laboratory of Bioelectronics Southeast University Nanjing 20096 Abstract Electrospun nylon 6 nanofibrous membrane based on solid membrane extraction-high performance liquid chromatography SME-HPLC for the determination of bisphenol A BPA in plastic bottled drinking water was performed. Important parameters that effect extraction efficiency such as eluting agent and its volume flow rate of sample sample volume ph of sample quality of the membrane the form of activation and the repeatedly employing of this membrane were optimized. Results indicated that 0 ml of water sample volume with ph of 8. 0 passed through nylon 6 nanofibrous membrane. 5 mg at flow rate of 3. 0 ml /min and only 300 μl eluent methanol was used. Each piece of this membrane would be used at least 6 times. Under the optimized conditions an excellent linear relationship in the range of 0. 2-20 μg /L with correlation coefficients of determination r 0. 9998 was obtained the limits of detection LOD about BPA was 0. 5 μg /L. The repeatabilities RSD intra-membrane and inter-membrane with nylon 6 nanofibrours membrane were all below 4. 5% n = 6. The proposed has been applied to the analysis of plastic bottled purified water of six different brands. Satisfactory spiked recoveries of 94. 95% were obtained. BPA was lower than 0. 30 μg / L. A comparison among the SME using nylon 6 nanofibrous membrane and other kinds of SPE sorbents used in literatures was carried out. All the results indicated that the nylon 6 nanofiboous membrane has great potential as a novel material for the enrichment and determination of BPA in water sample. Keywords Nylon 6 nanofibrours membrane Solid-membrane extraction Biphenol A Plastic bottled Drinking water High performance liquid chromatography Received 6 July 2009 accepted September 2009 櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋櫋 ~ 9 0 ~ 8 9 68. 00