微波辅助合成分子印迹聚合物用于萃取蜂蜜中的氯霉素

doi:10.7503/cjcu20140607

高等学校化学学报 ›› 2015, Vol. 36 ›› Issue (1): 67.doi: 10.7503/cjcu20140607

微波辅助合成分子印迹聚合物用于萃取蜂蜜中的氯霉素

陈海燕¹, 丁兰¹, 刘密兰²()

1.吉林大学化学学院, 2. 物理学院, 长春 130012

收稿日期:2014-07-02 修回日期:2014-12-23 出版日期:2015-01-10 发布日期:2014-12-23
作者简介:联系人简介: 刘密兰, 女, 高级工程师, 主要从事光谱及穆斯堡尔谱分析研究. E-mail: liuml@jlu.edu.cn
基金资助:
吉林省科技发展计划项目(批准号: 20120327)资助

Preparation of Molecularly Imprinted Polymers by Microwave-assisted Polymerization for the Extraction of Chloramphenicol from Honey^†

CHEN Haiyan¹, DING Lan¹, LIU Milan^2,^*()

1. College of Chemistry, 2. College of Physics, Jilin University, Changchun 130012, China

Received:2014-07-02 Revised:2014-12-23 Online:2015-01-10 Published:2014-12-23
Contact: LIU Milan E-mail:liuml@jlu.edu.cn
Supported by:
Supported by the Development Program of the Ministry of Science and Technology of Jilin Province, China(No. 20120327)

摘要/Abstract

摘要：

采用微波辅助法快速制备以氯霉素为模板分子的分子印迹聚合物. 将合成的聚合物作为吸附剂, 选择性分离和富集蜂蜜样品中的氯霉素, 并结合高效液相色谱-串联质谱法对萃取物进行分析. 对合成的分子印迹聚合物进行了表征, 考察了聚合物的吸附性能及其选择性, 并进行了Scatchard分析. 结果表明, 合成的聚合物为球形, 对氯霉素具有良好的识别能力, 最大表观结合量可达0.428 mmol/g. 该方法的线性范围为0.5~100 ng/g, 相关系数>0.999, 蜂蜜中氯霉素的检出限为0.13 ng/g, 6种蜂蜜样品中氯霉素的加标回收率范围为88%~93%.

关键词: 分子印迹聚合物, 微波辅助合成, 固相萃取, 氯霉素, 液相色谱-串联质谱法

Abstract:

The chloramphenicol imprinted polymers were prepared by means of microwave-assisted polymerization and applied for the separation and enrichment of chloramphenicol from honey. The polymers were applied as solid-phase extraction materials to extract and clean up the chloramphenicol in honey, followed by the liquid chromatography-tandem mass spectrometry(LC-MS/MS) analysis. The morphology of polymers was characterized by scanning electron microscope(SEM). The binding property and selectivity of polymers were evaluated and the Scatchard analysis was carried out. The polymers appeared to be spherical in shape and had a good selectivity. The apparent maximum binding amount of the polymers was 427.7 μmol/g. The detection limit of chloramphenicol was 0.13 ng/g. The linearity range and correlation coefficient of the method were 0.5—100 ng/g and 0.999, respectively. The recoveries of six spiked honey samples were in the range of 88%—93%. The proposed method has been successfully applied for the detection of chloramphenicol from honey.

Key words: Molecularly imprinted polymer, Microwave-assisted polymerization, Solid-phase extraction, Chloramphenicol, Liquid chromatography-tandem mass spectrometry

中图分类号:

O658.2

TrendMD:

陈海燕, 丁兰, 刘密兰. 微波辅助合成分子印迹聚合物用于萃取蜂蜜中的氯霉素. 高等学校化学学报, 2015, 36(1): 67.

CHEN Haiyan, DING Lan, LIU Milan. Preparation of Molecularly Imprinted Polymers by Microwave-assisted Polymerization for the Extraction of Chloramphenicol from Honey^†. Chem. J. Chinese Universities, 2015, 36(1): 67.

图/表 10

Fig.1 Chemical structures of chloramphenicol(A), florfenicol(B) and sulfamonomethoxine(C)

Table 1 MS parameters of chloramphenicol

Analyte	Precursor ion, m/z	Product ion, m/z	DP/V	EP/V	CEP/V	CE/eV	CXP/V
Chloramphenicol	321.1	257.1	-35	-8	-20	-20	-3
		152.1^*	-40	-8	-20	-25	-1

Fig.2 SEM image of MIPs

Fig.3 FTIR spectrum of MIPs

Fig.4 Binding isotherms(A) and Scatchard plot analysis of the binding of CAP onto the MIPs(B) and NIPs(C)

Fig.5 Evaluation of the MIPs(a1—c1) and NIPs(a2—c2) selectivity a1,a2. Chloramphenicol; b1,b2. florfenicol; c1,c2. sulfamonomethoxine.

Fig.6 Effect of flow rate on the recovery of chlo-ramphenicol(n=3)

Fig.7 Effect of pH on the recovery of chloramphenicol(n=3)

Fig.8 Effect of elution volume on the recovery of chloramphenicol(n=3)

Fig.9 LC-MS/MS extracted ion chromatograms of the blank(A) and spiked honey sample(0.5 ng/g)(B)

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微波辅助合成分子印迹聚合物用于萃取蜂蜜中的氯霉素

Preparation of Molecularly Imprinted Polymers by Microwave-assisted Polymerization for the Extraction of Chloramphenicol from Honey^†

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微波辅助合成分子印迹聚合物用于萃取蜂蜜中的氯霉素

Preparation of Molecularly Imprinted Polymers by Microwave-assisted Polymerization for the Extraction of Chloramphenicol from Honey†

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Preparation of Molecularly Imprinted Polymers by Microwave-assisted Polymerization for the Extraction of Chloramphenicol from Honey^†