新型磁性分子印迹聚合物的制备及其在氟喹诺酮类抗生素检测中的应用

doi:10.3724/SP.J.1123.2016.09023

摘要/Abstract

摘要：

建立了磁性分子印迹聚合物固相萃取与高效液相色谱联用同时检测环境水中4种氟喹诺酮类抗生素的研究方法。分别利用扫描电子显微镜、透射电子显微镜、X-射线衍射、傅里叶红外光谱、振动样品磁强计对合成的磁性分子印迹聚合物进行表征，对影响吸附实验的参数（包括吸附剂用量、吸附和解析时间、洗脱液种类、样品pH值）进行了考察和优化。在最佳的实验条件下，4种氟喹诺酮类抗生素的方法检出限为4.1~21.3 μg/L，方法定量限为13.7~71.0 μg/L，样品加标回收率为70.6%~103.6%。该方法快速、灵敏，能够满足环境水样中氟喹诺酮类抗生素的残留检测要求。

关键词: 磁性分子印迹聚合物, 氟喹诺酮类抗生素, 高效液相色谱, 环境水样, 吸附剂

Abstract:

This paper deals with a method based on magnetic molecularly imprinted polymers (MMIPs) as a sorbent. The method was used for simultaneous determination of fluoroquinolone antibiotics (ciprofloxacin, lomefloxacin, enoxacin, and norfloxacin) combined with high performance liquid chromatography (HPLC). MMIPs were characterized by different techniques (scanning electron microscopy, transmission electron microscopy, X-ray diffractometry, Fourier transform infrared spectrometry and vibrating sample magnetometry). Several parameters affecting the adsorption/desorption, including the amount of MMIPs, extraction and desorption times, desorption solvent, and sample pH, were investigated and optimized. Under the optimum conditions, the limits of detection (LODs) and the limits of quantification (LOQs) of the method were calculated to be 4.1-21.3 μg/L and 13.7-71.0 μg/L, respectively, and the recoveries of spiked samples ranged from 70.6% to 103.6%. The prepared MMIPs could be employed to selectively preconcentrate and determine fluoroquinolone antibiotics from environmental water samples.

Key words: environmental water samples, fluoroquinolone antibiotics, high performance liquid chromatography (HPLC), magnetic molecularly imprinted polymers (MMIPs), sorbent

中图分类号:

O658

佟育奎, 胡月, 夏琴飞, 黄玮, 田苗苗. 新型磁性分子印迹聚合物的制备及其在氟喹诺酮类抗生素检测中的应用[J]. 色谱, 2017, 35(3): 291-301.

TONG Yukui, HU Yue, XIA Qinfei, HUANG Wei, TIAN Miaomiao. Preparation of a novel magnetic molecularly imprinted polymer and its application for the determination of fluoroquinolone antibiotics[J]. Chinese Journal of Chromatography, 2017, 35(3): 291-301.

参考文献

[1] Pico Y, Andreu V. Anal Bioanal Chem, 2007, 387: 1287
[2] Fick J, Söderström H, Lindberg R H, et al. Environ Toxicol Chem, 2009, 28: 2522
[3] Kolpin D W, Furlong E T, Meyer M T, et al. Environ Sci Technol, 2002, 36: 1202
[4] Li L, Liu F, Chen H H, et al. Chinese Journal of Chromatography, 2013, 31(6): 567
[5] Vieno N, Tuhkanen T, Kronberg L. Water Res, 2007, 41: 1001
[6] Wang L, Zhong D L, Chen G C, et al. Chinese Journal of Chromatography, 2013, 31(10): 1010
[7] Poliwoda A, Krzyzak M, Wieczorek P P. J Chromatogr A, 2010, 1217: 3590
[8] Speltini A, Sturini M, Maraschi F, et al. Anal Bioanal Chem, 2012, 404: 1565
[9] Sturini M, Speltini A, Maraschi F, et al. J Chromatogr A, 2010, 1217: 7316
[10] Liu D, Ma J T, Jin Y, et al. J Sep Sci, 2015, 38: 134
[11] Benito-Pena E, Urraca J L, Sellergren B, et al. J Chromatogr A, 2008, 1208: 62
[12] Chen B, Wang W D, Huang Y M. Talanta, 2012, 88: 237
[13] Tan Y, Wei T X. Talanta, 2015, 141: 279
[14] Du B, Qu T T, Chen Z, et al. Talanta, 2014, 129: 465
[15] Mehdinia A, Dadkhah S, Kayyal T B, et al. J Chromatogr A, 2014, 1364: 12
[16] Chen F F, Shi Y P. Chinese Journal of Chromatography, 2013, 31(7): 626
[17] Chen W, Xue M, Xue F, et al. Talanta, 2015, 140: 68
[18] Hu X G, Fan Y N, Zheng Y, et al. Anal Chim Acta, 2012, 731: 40
[19] Mehdinia A, Kayyal T B, Jabbari A, et al. J Chromatogr A, 2013, 1283: 82
[20] Ma R T, Shi Y P. Talanta, 2015, 134: 650
[21] Qiu H, Fan L, Li X, et al. J Pharmaceut Biomed, 2013, 75: 123
[22] Lin Z Z, Zhang H Y, Li L, et al. React Funct Polym, 2016, 98: 24
[23] Chen L G, Zhang X P, Xu Y, et al. Anal Chim Acta, 2010, 662: 31
[24] Zhang Y, Liu R, Hu Y, et al. Anal Chem, 2009, 81: 967
[25] Tian M M, Chen D X, Sun Y L, et al. RSC Adv, 2013, 3: 22111
[26] Tian M M, Zou Y C, Zhou S Y, et al. J Chromatogr B, 2015, 1007: 1
[27] Zhao L, Wu R A, Han G H, et al. J Am Soc Mass Spectr, 2008, 19: 1176
[28] Fang L J, Chen S J, Zhang Y, et al. J Mater Chem, 2011, 21: 2320
[29] Mosbach K, Ramstrom O. J Biotechnol, 1996, 14: 163
[30] Piletsky S A, Karim K, Piletska E V, et al. Analyst, 2001, 126: 1826
[31] Baggiani C, Giraudi G, Giovannoli C, et al. J Chromatogr A, 2000, 883: 119
[32] Zhou S Y, Li Z, Lv X J, et al. Analyst, 2015, 140: 5944
[33] Zhou Y S, Zhou T T, Jin H, et al. Talanta, 2015, 137: 1
[34] Paul T, Liu J Y, Machesky M L, et al. J Colloid Interf Sci, 2014, 428: 63
[35] Lv Y K, Yang L, Liu X H, et al. Anal Methods, 2013, 5: 1848
[36] Luaces M D, Urraca J L, Pérez-Conde M C, et al. Microchem J, 2013, 110: 458
[37] Liu X, Wang X C, Tan F, et al. Anal Chim Acta, 2012, 727: 26
[38] Tang W J, Zhao T, Zhou C H, et al. Anal Methods, 2014, 6: 3309
[39] Sousa J, Alves G, Campos G, et al. J Chromatogr B, 2013, 930: 104
[40] Wang Y P, Sun Y, Gao Y, et al. Talanta, 2014, 119: 268