MIP. 5 mmol /L Tris-HCl mol /L NaCl 24 h b 3. 2 MIP NaTFPB

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1 FENXI HUAXUE Chinese Journal of Analytical Chemistry ~ 358 DOI /SP. J * "8 mol /L "7 ~ "4 mol /L mv /decade 98% ~ 107% 3 min HPLC 2 - GC-MS 3 4 ELISA 5 HPLC GC-MS ELISA 6 ~ 8 9 MIPs 10 MIPs MIPs MIPs PXSJ-216 DU-800 / Beckman S-4800 MAA MMA TRIM 80 DVB 80 PVC o-npoe 3 5- NaTFPB THF Sig No No. JQ * wqin@ yic. ac. cn

2 3 355 ma-aldrich AIBN MAA TRIM DVB 80 THF AIBN Pall Cascada MΩ cm 0. 1 mmol /L pk a = mmol /L Tris-HCl ph mmol 2. 5 mmol MAA mmol MMA 40 ml 1 h 1 mmol TRIM 0. 4 mmol DVB 0. 5 mmol AIBN 10 min h V /V λ = 245 nm NIP MAA MMA 2. 3 MIP NIP NaTFPB o-npoe PVC 5. 0% w /w MIP NIP 1. 0% w /w NaTFPB 62. 6% w /w o-npoe 31. 4% w /w PVC mg 3. 5 ml THF 2 h 3. 6 cm 12 h 9 mm THF "4 mol /L 5 mmol /L Tris-HCl ph h mol /L NaCl 24 h 2. 4 Ag /AgCl PXSJ-216 Hg 2 Cl 2 Hg KCl PVC Ag AgCl 3 mol /L KCl Henderson Debye-Hückel MIP NIP MIP NIP 1a 12 MIP 0. 5 ~ 1. 0!m MIP PVC MIP 1b NIP MIP 3. 2 MIP NaTFPB PVC MIP MIP MAA MMA NaTFPB PVC

3 Fig. 1 SEM images of obtained a clenbuterol-mip and b NIP beads 1 1% MIP MIP MIP 5% MIP o-npoe ε r = DOS ε r = 4. 8 DOP ε r = % w /w PVC 62. 7% w /w NPOE 1% w /w NaTFPB 5% w /w MIP 1 Table 1 Influence of membrane composition on electrode response PVC Plasticizer NPOE DOS DOP NaTFPB MIP Linear range mol /L Slope a mv /decade "6 ~ 1 10 " ± "7 ~ 1 10 " ± "7 ~ 1 10 " ± "6 ~ 1 10 " ± "6 ~ 1 10 " ± "7 ~ 1 10 " ± "7 ~ 1 10 " ± 0. 5 a 3 ± Average from three measurements ± standard deviation NPOE Nierophenyl octyl ether DOP Dioctyl phthalate NaTFPB Sodiom tetrakis 3 5-bis trifluoro-methyl phenyl borate ph ph 1 ~11 2 ph 7. 0 ~ 8. 5 ph > 8. 5 ph ph < MIP 2 ph 0. 1 mmol /L "7 ~ "4 mol /L mv /decade "8 mol /L Fig. 2 Effect of sample ph on the electrode response MIP NIP of 0. 1 mmol /L clenbuterol

4 3 357 MIP MIP NIP Nicolskii-Eisenman 3 K pot J 15 I 2 Fig. 3 Calibration curves for clenbuterol-mip NIP and blank membranes Na + K + Ca 2 + Mg 2 + NH + 4 logk pot I J "7. 57 "5. 94 "7. 43 "7. 78 "6. 17 "2. 50 Na + K + 2 n = 3 Table 2 Potentiometric selectivity coefficients for the MIPbased clenbuterol ISE n = % Interfering ion logk Interfering ion logk 4 Na + "7. 57 "6. 28 a Cu 2 + " "5 ~ 1 10 "4 mol /L K + "5. 94 "4. 96 a Zn 2 + " s 1 H + "6. 86 Ractopamine ion " "5 ~1 10 "4 mol /L 1 10 "4 ~ Ca 2 + "7. 43 Ethylenediamine ion "6. 06 Mg 2 + "7. 78 NH 4 + " "5 mol /L a NIP Values in parentheses are t he selectivity coefficients for NIP membrane electrode % !m 3 98% ~ 107% 3 min 3 Table 3 Application of the proposed electrode to determination of clenbuterol in pig urine samples spiked with different amounts of clenbuterol Sample Added Found n = 3 a # # # # Recovery % 4 a # Average from three measurements ± standard deviation Fig. 4 Potential response of the MIP based ISE

5 References 1 van Vyncht G Preece S Gaspar P Maghuin-Rogister G Depauw E. J. Chromatogr. A ~ 49 2 WU Yin-Liang YANG Ting SHAN Ji-Hao HUANGFU Wei-Guo. Chinese J. Anal. Chem ~ ~ WU Yin-Liang LI Xiao-Wei LIU Su-Ying SHEN Jian-Zhong YANG Ting. Chinese J. Anal. Chem ~ ~ HU Hua-Jun FU Tao ZHANG Ming-Zhou HONG Zhi CHEN Zong-Lun LIU Jun. Chinese J. Anal. Chem ~ ~ Roda A Manetta A C Piazza F Simoni F Lelli R. Talanta ~ Sokalski T Ceresa A Zwickl T Pretsch E. J. Am. Chem. Soc ~ Bakker E Pretsch E. Angew. Chem. Int. Ed ~ Ding J W Qin W. J. Am. Chem. Soc ~ Haupt K Mosbach K. Chem. Rev ~ HU Yu-Fang ZHANG Zhao-Hui ZHANG Hua-Bin YU Xiao-Xiao YAO Shou-Zhuo. Chem. J. Chinese Universities ~ ~ Yoshimatsu K Reimhult K Krozer A Mosbach K Sode K Ye L. Anal. Chim. Acta ~ Liang R N Song D A Zhang R M Qin W. Angew. Chem. Int. Ed ~ Shan J Pan C Zhang J Niu W. Acta Chromatogr ~ Bakker E. J. Electrochem. Soc L83 ~ L85 15 Smith M J Manahan S E. Anal. Chem ~ 839 Potentiometric Sensor Based on Molecularly Imprinted Polymer for Rapid Determination of Clenbuterol in Pig Urine LIANG Rong-Ning 1 GAO Qi 1 2 QIN Wei * 1 1 Chinese Academy of Sciences and Shandong Provincial Key Laboratory of Coastal Zone Environmental Processes Yantai Institute of Coastal Zone Research Chinese Academy of Sciences Yantai China 2 Graduate University of Chinese Academy of Sciences Beijing China Abstract A polymeric membrane ion-selective electrode for the determination of clenbuterol is described. It is based on a molecularly imprinted polymer MIP as an ionophore for molecular recognition which can be synthesized by precipitation polymerization using clenbuterol hydrochloride as a template molecule. Under the optimized conditions the proposed membrane electrode exhibits Nernstian response to the protonated clenbuterol over the concentration range of " "4 mol /L with a slope of mv /decade and the detection limit is "8 mol /L. The MIP-based sensor shows excellent selectivity rapid response time and satisfactory long-term stability. The potentiometric sensor has been successfully applied to determine the clenbuterol in pig urine samples with recoveries between 98% and 107% and an analytical time of less than 3 min. Keywords Molecularly imprinted polymer Potentiometric sensor Clenbuterol Received 10 August 2011 accepted 22 September 2011

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