在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留

doi:10.3724/SP.J.1123.2015.11020

色谱 ›› 2016, Vol. 34 ›› Issue (4): 422-428.DOI: 10.3724/SP.J.1123.2015.11020

在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留

许旭^1,2, 肖远灿¹, 耿丹丹^1,2, 皮立¹, 董琦¹, 胡风祖¹

1. 中国科学院西北高原生物研究所, 青海西宁 810008;
2. 中国科学院大学, 北京 100049

收稿日期:2015-11-12 出版日期:2016-04-08 发布日期:2012-11-16
通讯作者: 肖远灿
基金资助:
中国科学院仪器功能开发技术创新项目(Ig201308);中国科学院知识创新工程重要方向项目(KSCX2-EW-J-26);青海省科技计划项目(2015-ZL-Y23);青海省科技平台建设项目(2012-T-Y19).

Simultaneous determination of 16 sulfonamide residues in beef by high performance liquid chromatography-fluorescence detection with online post-column derivatization

XU Xu^1,2, XIAO Yuancan¹, GENG Dandan^1,2, PI Li¹, DONG Qi¹, HU Fengzu¹

1. Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810008, China;
2. University of Chinese Academy of Sciences, Beijing 100049, China

Received:2015-11-12 Online:2016-04-08 Published:2012-11-16
Supported by:
Instrument Function Development and Technology Innovation Project of Chinese Academy of Sciences (No. Ig201308);Knowledge Innovative Program of Chinese Academy of Sciences (No. KSCX2-EW-J-26);Science and Technology Plan Project of Qinghai Province (No. 2015-ZL-Y23);Science and Technology Platform Construction Project of Qinghai Province (No. 2012-T-Y19).

摘要/Abstract

摘要：

在考察了荧光胺、邻苯二甲醛、异硫氰酸荧光素和2,3-萘二醛等对磺胺类药物衍生效果的基础上,建立了采用改良QuEChERS方法进行样品前处理,荧光胺在线柱后衍生,高效液相色谱-荧光检测法测定牛肉中16种磺胺残留量的方法。牛肉样品经1%(v/v)乙酸乙腈溶液提取,改良QuEChERS方法净化后取上清液进样,与荧光胺柱后在线衍生,荧光检测器检测。实验结果表明,16种磺胺类药物在0.024~2.533 mg/L范围内线性关系良好,相关系数(r)大于0.992,检出限为1.6~8.2 μg/kg,平均加标回收率范围为66.6%~109.5%,相对标准偏差为0.9%~9.9%。该方法快速简便、灵敏度高、净化效果好,可用于牛肉中16种磺胺类药物的快速测定。

关键词: QuEChERS, 高效液相色谱-荧光检测法, 磺胺类药物, 牛肉, 荧光胺, 在线柱后衍生

Abstract:

In this study, we investigated the effects of the four kinds of derivatization reagents, including fluorescamine, o-phthaladehyde, fluorescein isothiocyanate isomer and 2, 3-naphthalenedicarboxaldehyde. A high performance liquid chromatography with fluorescence detection method for the rapid determination of 16 sulfonamide residues in beef was developed by using improved QuEChERS method for sample pretreatment and fluorescamine for online post-column derivatization. The beef samples were extracted with acetonitrile containing 1%(v/v) acetic acid, cleaned-up by QuEChERS method, injected for online post-column derivatization with fluorescamine, and then analysed with fluorescence detection. Under the optimized conditions of QuEChERS and chromatography, the 16 sulfonamide residues showed good linearities in the range of 0.024-2.533 mg/L with the correlation coefficients (r) higher than 0.992. The limits of detection of the method were 1.6 to 8.2 μg/kg. The average recoveries of the 16 sulfonamide residues were in the range of 66.6%-109.5% with the relative standard deviations from 0.9% to 9.9%. The method has the advantages of rapidity, simplicity, high sensitivity and better purification effect. It is suitable for the rapid determination of the sulfonamide residues in beef.

Key words: beef, fluorescamine, high performance liquid chromatography-fluorescence detection (HPLC-FLR), online post-column derivatization, QuEChERS, sulfonamides

中图分类号:

O658

许旭, 肖远灿, 耿丹丹, 皮立, 董琦, 胡风祖. 在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留[J]. 色谱, 2016, 34(4): 422-428.

XU Xu, XIAO Yuancan, GENG Dandan, PI Li, DONG Qi, HU Fengzu. Simultaneous determination of 16 sulfonamide residues in beef by high performance liquid chromatography-fluorescence detection with online post-column derivatization[J]. Chinese Journal of Chromatography, 2016, 34(4): 422-428.

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在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留

Simultaneous determination of 16 sulfonamide residues in beef by high performance liquid chromatography-fluorescence detection with online post-column derivatization

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