729 NHS EDC 5% w /V PEI Tetramethylrhodamine-5-isothiocyanate TRITC N- 2- -N'- 2- HEPES U D Sigma-ldrich SDS 5 mmol /L 5 mmol /L HEPE

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1 43 25 FENXI HUXUE Chinese Journal of nalytical Chemistry 728~ 734 DOI.895 /j.issn * * EDC /NHS 3- P P P-P QCM FM >5 μg /ml ~ 3 4~ 7 QCM / 8 9 FM 8 QCM FM 2 2. Nicolet is5 UV-36 ESCLab 25XiX XPS Q-Sense E4 QCM Nanoscope IIIa Digital Instruments P M n 3 3- P N Nos No. ZR24M25 No * qf_qw@ 63.com huawangqfnu@ 26.com

2 729 NHS EDC 5% w /V PEI Tetramethylrhodamine-5-isothiocyanate TRITC N- 2- -N'- 2- HEPES U D Sigma-ldrich SDS 5 mmol /L 5 mmol /L HEPES Millipore 2.2 P-P P-P EDC /NHS P P 2 3 mmol P HEPES ph ml.6 mol /L P 4 ml.3 mol /L NHS EDC 2 h P-P 2.3 PEI /P-P 3.7 mm 5. mm 5 μl % SDS 3 μl Piranha H 2 SO 4-3% H 2 O V /V min 5 μl PEI.2 mol /L NaCl 2 min 3 5 μl P-P.2 mol /L NaCl QCM PEI /P-P 3 3. P-P EDC NHS P-P cm! P cm! P-P 36 cm! O 438 cm! P P P-P XPS P-P 3 N P P 38% P-P NH 2 n CO EDC/NHS ph8.5 2 h CO HN n- CO Fig. Synthetic scheme of poly acrylic acid -phenylboronic acid P-P Wavenumber (cm - ) P-P 3.2 PEI /P-P Fig.2 FTIR spectra of 3-aminophenylboronic acid hemisulfate P and P-P P-P Transmittance P 鄄 P 295 P ph 9. - QCM FM TRITC PEI 4 55 nm

73 43 25 Intensity (a.u.) 2 Os 5 Ns 5 2 8 6 4 inding energy ( ev) Cs CO HN s 2 CO n- 3 Fig.3 P-P XPS XPS spectra of P-P QCM 5 FM 6 2 4 6 PEI /P-P bsorbance.7.6.5.4.3.2. 6-2 -4-6 -8 PEI P 鄄 P 4 45 5 55 6 65 7 姿 (nm) - 2 4 6 8 2 ssmbly layer number 4 Fig.

3 Intensity (a.u.) 2 Os 5 Ns inding energy ( ev) Cs CO HN s 2 CO n- 3 Fig.3 P-P XPS XPS spectra of P-P QCM 5 FM PEI /P-P bsorbance PEI P 鄄 P 姿 (nm) ssmbly layer number 4 Fig.4 PEI /P-P n UV-vis spectra and frequency shift observed during assembly of PEI /P-P n multilayer PEI Poly ethyleneimine. C 滋 m 滋 m 2 3 滋 m 4 5 PEI /P-P n 5 μm 5 μm PEI / P-P 2 PEI /P-P 4 C PEI /P-P 6 Fig.5 FM height images of PEI /P-P 2 multilayer PEI /P-P 4 multilayer and C PEI /P-P 6 multilayer

4 PEI /P-P QCM μg /ml 6 7 P μg /ml μg /ml 3 μg /ml 5 μg /ml lanck bilayer 2 bilayer 3 bilayer 4 bilayer 5 bilayer 7 bilayer 滋 g/ml 5 滋 g/ml 滋 g/ml 3 滋 g/ml 5 滋 g/ml PEI /P-P μg /ml QCM Fig. 6 Time courses of frequency shift observed during recognition of PEI /P-P n multilayer to glucose at concentration of μg /ml 7 PEI /P-P 4 QCM Fig. 7 Time courses of frequency shift observed during recognition of PEI /P-P 4 multilayer to glucose with different concentrations FM 8 R a ~ 3.52 nm PEI /P-P 3.4 PEI /P-P PEI /P-P U D U D ph 8. ph. ph 8. 2

732 43 5. nm 25. nm nm 5. nm C D 25. nm nm 8 PEI /P-P 4 μm μm C D Fig.

5 nm 25. nm nm 5. nm C D 25. nm nm 8 PEI /P-P 4 μm μm C D Fig.8 FM height images of PEI /P-P 4 multilayer before recognition to glucose FM phase images of PEI /P-P 4 multilayer before the recognition to glucose C FM height images of PEI /P-P 4 multilayer in recognition equilibrium to glucose and D FM phase images of PEI /P- P 4 multilayer in recognition equilibrium to glucose PEI /P- 滋 g/ml glucose P 滋 g/ml fructose 滋 g/ml mannose -2 滋 g/ml galactose QCM PEI /P-P 4 μg /ml QCM Fig.9 Time courses of frequency shift observed during P-P recognition of PEI /P-P 4 multilayer to glucose P fructose mannose and galactose with same concentration QCM FM of μg /ml

6 滋 g/ml glucose 3 滋 g/ml glucose+ 滋 g/ml + 滋 g/ml U 滋 g/ml + 滋 g/ml U 滋 g/ml glucose 3 滋 g/ml glucose+ 滋 g/ml D 滋 g/ml D PEI /P-P 4 3 μg /ml μg /ml μg /ml U μg /ml D QCM Fig. Time courses of frequency shift observed during the recognition of PEI /P-P 4 multilayer to glucose concentration of 3 μg /ml in the absence and the presence of ascorbic acid uric acid U in the absence and presence of dopamine D ph. ph new once recycled twice recycled PEI /P-P 4 ph 8. ph. QCM PEI /P-P 4 3 μg /ml QCM Fig. Time courses of frequency shift observed PEI /P-P 4 multilayer recognized with glucose at ph 8. and ph. respectively during the recognition of PEI /P-P 4 multilayer newly fabricated that recycled once and twice to glucose at the concentration of 3 μg /ml respectively References Kim K T Cornelissen J J L M Nolte R J M van Hest J C M. J. m. Chem. Soc LIU in SUN Xiang-Ying XU Jin-Rui. Chinese J. nal. Chem 分析化学, Watahiki R Sato K Suwa K Niina S Egawa Y Seki T nzai J I. J. Mater. Chem Decher G. Science Qi W Duan L Wang K W Yan X H Cui Y. He Q Li J. dv. Mater Qi W Xue Z Yuan W Wang H. J. Mater. Chem Qi W Yuan W Yan J Wang H. J. Mater. Chem Yamashita K Kikkawa Y Kurokawa K. Doi Y. iomacromolecules DU in-yang FN Xiao CO Zheng GUO Xiao-Lei. Chinese J. nal. Chem 分析化学, LI Jing WNG Er-Kang. Chinese J. nal. Chem 分析化学,

7 Yao H Q Chang F W Hu N F. Electroch. cta Levy T Déjugnat C Sukhorukov G. dv. Funct Mater Quartz Crystal Microbalance and tomic Force Microscopy for Study of Carbohydrate-sensitive Multilayers Composed of Pheylboronic cid Polymers YUN Wen-Jing ZHONG Tong YN Jing XUE Zhong-Yuan QI Wei * WNG Hua * Key Laboratory of Life-Organic nalysis Key Laboratory of Pharmaceutical Intermediates and nalysis of Natural Medicine School of Chemistry and Chemical Engineering Qufu Normal University Qufu China bstract oronic acids and their derivatives have been widely used in carbohydrate-sensitive materials because they can selectively bind 2-and 3-diol compounds including sugars to form cyclic boronate esters. In this work pheylboronic acid P moieties were grafted onto the backbone of poly acrylic acid P through the condensation reaction between aminopheyl-boronic acid and carboxylic acid group of P in the presence of EDC /NHS designed as P-P. Then the resulting P-P were assembled with poly ethyleneimine PEI to form P-P multilayer films. The sensing performance of the PEI /P-P film to carbohydrate > 5 μg /ml including glucose fructose mannose and galactose has been investigated by combination of the complementary techniques of quartz crystal microbalance QCM and atomic force microscopy FM. It was demonstrated that the multilayer showed higher sensitivity to fructose than glucose mannose and galactose. The interferences of ascorbic acid uric acid and dopamine to the recognition of glucose can be avoided and the multilayer sensor with excellent long term stability can be recycled by changing ph value of buffer solutions. This system may be potential in realization of high selectivity and high sensitivity sensing system for probing carbohydrate. Keywords Pheylboronic acid Layer-by-layer assembly Carbohydrate-sensitive Quartz crystal microbalance tomic force microscopy Received July 25 accepted 5 October 25 This work was supported by the National Natural Science Foundation of China Nos and the Natural Science Foundation of Shandong Province China No. ZR24M25 and Student Research training Program of Qufu Normal University No 櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫櫫

ph ph ph Langmuir mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 3 CO 2-3 PO mg /L 5 p

ph ph ph Langmuir mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 3 CO 2-3 PO mg /L 5 p 1 2 1 2 3 1 2 1. 100054 2. 100054 3. 100036 ph ph ph Langmuir 166. 67 mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 4 5. 00 mg /L 5 ph doi 10. 13928 /j. cnki. wrahe. 2017. 03. 017 TV213. 4 + TU991. 26 + 6 A 1000-0860