分子印迹固相萃取-高效液相色谱法测定牛奶中四环素类抗生素残留

doi:10.3969/j.issn.1004-1524.2018.02.19

浙江农业学报 ›› 2018, Vol. 30 ›› Issue (2): 314-322.DOI: 10.3969/j.issn.1004-1524.2018.02.19

分子印迹固相萃取-高效液相色谱法测定牛奶中四环素类抗生素残留

付珍珍, 曾月, 李增威, 何利, 周康, 刘书亮, 邹立扣, 敖晓琳, 陈姝娟^*

四川农业大学食品学院,四川雅安 625014

收稿日期:2017-07-12 出版日期:2018-02-20 发布日期:2018-02-11
通讯作者: 陈姝娟,E-mail:chenshujuan1@163.com
作者简介:付珍珍(1992—),女,四川资阳人,硕士研究生,研究方向为食品加工与安全。E-mail:530410137@qq.com
基金资助:
四川省教育厅项目(15ZB0018)

Determination of tetracycline antibiotics residues in milk by molecularly imprinted solid phase extraction-high performance liquid chromatography

FU Zhenzhen, ZENG Yue, LI Zengwei, HE Li, ZHOU Kang, LIU Shuliang, ZOU Likou, AO Xiaolin, CHEN Shujuan^*

College of Food Science, Sichuan Agricultural University, Ya'an 625014, China

Received:2017-07-12 Online:2018-02-20 Published:2018-02-11

摘要/Abstract

摘要： 采用分子印迹技术合成四环素类分子印迹聚合物,以其为填料制备固相萃取柱,运用高效液相色谱法测定牛奶中的四环素类抗生素。具体地,以盐酸强力霉素为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用沉淀聚合法在丙酮-乙腈混合溶液中制备具有特异性吸附能力的分子印迹聚合物,通过高效液相色谱仪检测其吸附四环素类抗生素的能力,并将其作为填料制备固相萃取柱,用于牛奶中四环素类抗生素残留检测。结果显示,四环素类抗生素在0.05~10.0 μg·mL^-1范围内线性良好,加标回收率为79.4%~86.3%,相对标准偏差均小于3.8%,准确性较好。四环素和土霉素的检出限为0.02 μg·mL^-1,金霉素的检出限为0.05 μg·mL^-1,检测灵敏度高,特异性识别能力强。

关键词: 分子印迹聚合物, 四环素类抗生素, 固相萃取, 检测方法

Abstract: Molecularly imprinted technology (MIT) was used for the synthesis of tetracyclines molecularly imprinting polymers (MIPs), which were used as the filler in the preparation of solid phase extraction column. Then high performance liquid chromatography (HPLC) was applied to determine the tetracyclines residues in milk. The MIPs with specific adsorption ability were synthesized by precipitation polymerization in acetone acetonitrile mixed solution, with doxycycline hydrochloride (DC) as the template molecule, methacrylic acid (MAA) as the function monomers and ethylene glycol dimethyl acrylic ester (EGDMA) as the crosslinking agent. Their ability of adsorbing tetracycline antibiotics was detected by HPLC, and the selected MIPs were used as filler to prepare a solid phase extraction column for the detection of tetracycline antibiotics residues in milk. It was shown that the tetracycline antibiotics presented a good linear correlation within 0.05-10.0 μg·mL^-1 and the recovery rates of tetracyclines were around 79.4%-86.3%, and the relative standard deviations were all less than 3.8%. The detection limits were 0.02 μg·mL^-1 for tetracycline and oxytetracycline, and was 0.05 μg·mL^-1 for chlortetracycline. The method was accurate, sensitive and specific.

Key words: molecular imprinted polymers, tetracycline antibiotics, solid phase extraction, determination method

中图分类号:

付珍珍, 曾月, 李增威, 何利, 周康, 刘书亮, 邹立扣, 敖晓琳, 陈姝娟. 分子印迹固相萃取-高效液相色谱法测定牛奶中四环素类抗生素残留[J]. 浙江农业学报, 2018, 30(2): 314-322.

FU Zhenzhen, ZENG Yue, LI Zengwei, HE Li, ZHOU Kang, LIU Shuliang, ZOU Likou, AO Xiaolin, CHEN Shujuan. Determination of tetracycline antibiotics residues in milk by molecularly imprinted solid phase extraction-high performance liquid chromatography[J]. , 2018, 30(2): 314-322.

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分子印迹固相萃取-高效液相色谱法测定牛奶中四环素类抗生素残留

Determination of tetracycline antibiotics residues in milk by molecularly imprinted solid phase extraction-high performance liquid chromatography

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