38 2010 1 FENXI HUAXUE Chinese Journal of Analytical Chemistry 1 67 ~ 71 * 361005 - ph 3 1. 0 ~ 200 μg /L LOD S /N = 3 0. 13 ~ 0. 66 μg /L LOQ S /N = 10 0. 44 ~ 2. 19 μg /L 3 37. 8% ~ 101. 1% A 1 Alkylphenols Aps 1 A Bisphenol A BPA A BPA OP NP N- 2 nonylphenol NP octyphenol OP 2008 10 18 BPA BPA OP NP 3 4 5 6 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 11 12 SBSE Polydimethylsiloxane PDMS SPME 25 ~ 250 ml 11 SBSE 13 SPME 50 14 SBSE PDMS PDMS 11 15 1 Stir bar for sorption extraction based on monolithic material SBSEM 16 ~ 19 SBSE SBSEM 2009-07-15 2009-09-26 No. 20805039 No. 2006F3117 * E-mail hxj@ xmu. edu. cn
68 38 N- - BPA OP NP ph HPLC- DAD 3 2 2. 1 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- - 1. 0 mm 12 BPA 99% TCI OP 99. 7% NP 99% Augsburg Tedia Milli-Q Millipore 2. 2 2. 5 mg 25 ml 100 mg /L 4 0. 45 μm 2. 3 Kromasil LC-18 250 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 2. 4 100 ml 250 ml 200 r /min 3. 0 ml 0. 5 ml 3 3. 1 3. 1. 1 1 1 0. 5 h 1. 5 h 1. 5 h BPA OP NP 1. 5 h 1. 5 h 1. 0 h SBSEM 1. 0 h 3. 1. 2 17 ~ 20 1 SBSEM Fig. 1 Effect of extraction time on extraction efficiency 1. A Bisphenol A BPA 2. Nonyphenol NP NaCl 3. Octyphenol OP 0 0. 05 0. 10 0. 15 0. 20 0. 25 g /ml 2a NaCl 0 ~ 0. 05 g /ml SBSEM
1 69 NaCl NaCl 16 ~ NaCl 19 2a BPA NP NaCl 0. 05 g /ml OP NaCl 0. 10 g /ml 0. 05 g /ml NaCl 0. 05 g /ml 3. 1. 3 ph ph 2. 0 11. 0 2b BPA ph = 7. 0 OP ph = 4. 0 ph = 7. 0 NP ph = 3. 0 ph = 7. 0 3 ph ph 7. 0 2 Fig. 2 a ph b Effect of ionic strength a and ph value b on extraction efficiency 1. A BPA 2. OP 3. NP 3. 2 1 1 3 LOD S /N = 3 0. 13 ~ 0. 66 μg /L LOQ S /N = 10 0. 44 ~ 2. 19 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 ~ 200 0. 9994 0. 13 0. 44 1. 9 9. 6 OP 3. 0 ~ 200 0. 9881 0. 43 1. 44 8. 8 3. 1 NP 3. 0 ~ 200 0. 9967 0. 66 2. 19 8. 8 1. 3 * Spiked level includes 1. 0 3. 0 5. 0 10. 0 50. 0 100. 0 200. 0 μg /L 3. 3 SBSEC 2 100 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 8. 08 10 2 1. 85 10 4 2. 00 10 4 SBSEM 1. 15 10 5 5. 91 10 4 4. 03 10 4
70 38 - SBSEM 16 3. 4 SBSEM HPLC-DAD 3 3 1. 41 μg /L BPA NP LOQ 3 1. 33 μg /L BPA 3 OP 3 3 10 μg /L 3 3 54. 4% ~ 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- 37. 8% ~ 101. 1% 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 0. 00 1. 41 ND ND 10. 00 9. 67 4. 97 3. 50 88. 8 ± 5. 5 81. 1 ± 6. 9 54. 4 ± 3. 0 100. 00 80. 2 90. 1 39. 6 81. 6 ± 1. 8 78. 0 ± 6. 9 37. 8 ± 3. 7 0. 00 ND ND 1. 44 10. 00 9. 09 6. 53 9. 73 90. 8 ± 8. 4 96. 5 ± 9. 0 99. 4 ± 6. 2 100. 00 76. 3 105. 9 74. 2 78. 4 ± 2. 0 91. 2 ± 2. 1 67. 6 ± 9. 8 0. 00 1. 33 ND ND 10. 00 9. 15 4. 41 6. 07 84. 1 ± 9. 1 75. 6 ± 9. 9 85. 2 ± 4. 9 100. 00 98. 9 96. 1 68. 0 101. 1 ± 5. 4 83. 0 ± 9. 4 64. 2 ± 8. 8 References 1 REN Ren CHEN Ming WU Shao-Hua ZHANG Shu-Fen WANG Gui-Hua. J. Beijing Univ. Tech. 2004 30 3 22 ~ 24 2 Renner R. Envrion Sci. Technol. 1997 31 7 316 ~ 320 3 SHAO Bing HAN Hao LI Dong-Mei ZHAO Rong MENG Juan MA Ya-Lu. Chinese Journal of Chromatography 2005 23 4 362 ~ 365 4 SHAO Bing GAO Ying-Xin HAN Hao ZHAO Rong MENG Juan WU Guo- Hua. Environ. Chem. 2005 24 5 483 ~ 484 5 Ballesteros O Zafra A Naval on A V lchez J L. J. Chromatogr. A 2006 1121 154 ~ 162 6 L Gang WANG Li-Bing LIU Jun ZHANG Shu-Fen. Chinese J. Anal. Lab. 2008 9 78 ~ 80 7 XIAO Shang-You WANG Jie-Feng XIA Zhi-Ning MU Xiao-Jing. Chinese J. Anal. Chem. 2009 37 8 1193 ~ 1196
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