食品科学

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分散固相萃取净化-气相色谱法测定水产品中氯霉素和氟苯尼考

胡红美1,郭远明1,*,雷 科2,张小军1,严忠雍1,何依娜1,尤炬炬1,刘 琴1   

  1. 1.浙江省海洋水产研究所 浙江省海水增养殖重点实验室,浙江 舟山 316100;
    2.浙江海洋学院水产学院,浙江 舟山 316000
  • 出版日期:2014-04-25 发布日期:2014-05-13
  • 通讯作者: 郭远明
  • 基金资助:

    浙江省科技计划项目(2012F30021;2012F30026);
    浙江省“农产品安全标准与检测技术”重点科技创新团队项目(2010R50028);浙江省自然科学基金项目(LQ13C200004)

Determination of Chloramphenicol and Florfenicol in Fishery Products by Using Dispersive Solid Phase Extraction and Gas Chromatography

HU Hong-mei1, GUO Yuan-ming1,*, LEI Ke2, ZHANG Xiao-jun1, YAN Zhong-yong1, HE Yi-na1, YOU Ju-ju1, LIU Qin1   

  1. 1. Key Laboratory of Mariculture and Enhancement of Zhejiang Province, Marine Fishery Institute of Zhejiang Province,
    Zhoushan 316100, China; 2. School of Fishery, Zhejiang Ocean University, Zhoushan 316000, China
  • Online:2014-04-25 Published:2014-05-13
  • Contact: GUO Yuan-ming

摘要:

建立测定水产品中氯霉素和氟苯尼考的气相色谱-电子捕获检测方法。样品通过乙酸乙酯萃取、正己烷初 步净化后,经过分散固相萃取进一步净化、硅烷化试剂衍生,再采用气相色谱-电子捕获法检测、外标法定量。 结果表明:氯霉素、氟苯尼考分别在1.5~100 μg/L、6~400 μg/L范围内,组分含量与峰面积呈线性相关,相关 系数分别为0.998 1和0.999 7,检出限分别为0.1、0.3 μg/kg。氯霉素和氟苯尼考在不同基质的水产品(鲫鱼、青 蟹、南美白对虾)中不同加标水平回收率分别为82%~106%、87%~111%和91%~98%,相对标准偏差分别为 2.3%~4.9%、2.4%~4.5%和1.4%~4.1%(n=5)。本方法基体干扰小、线性范围宽,灵敏度、准确度、精密度能满 足水产品中氯霉素类药物的含量分析。

关键词: 分散固相萃取, 气相色谱-电子捕获检测法, 水产品, 氯霉素类药物

Abstract:

An efficient, sensitive, and low matrix interference method for the determination of chloramphenicol (CAP) and
florfenicol (FF) in fishery products using gas chromatography-electron capture detector (GC-ECD) has been developed.
Samples were treated by extraction with ethyl acetate and n-hexane purification. Further cleanup of the extracts was
processed by a modified dispersive solid phase extraction procedure. Then, the purified solutions were derivatized with slilyl
reagents. The linearity of the method ranged from 1.5 to 100 μg/L for CAP, and from 6 to 400 μg/L for FF, with correlation
coefficients ranging between 0.998 1 and 0.999 7. The limits of detection were 0.1–0.3 μg/kg. The recoveries of spiked CAP
and FF with external calibration method at different concentration levels in different sample matrixes (crucian, blue crab,
and Penaeus vannawei) were 82%–106%, 87%–111%, and 91%–98%, respectively, with relative standard deviations of
2.3%–4.9%, 2.4%–4.5%, and 1.4%–4.1% (n = 5), respectively. Thus it is concluded that this method can be successfully
applied for the determination of choramphenicols (CAPs) in fishery products.

Key words: dispersive solid phase extraction, gas chromatography-electron capture detector, fisher products, choramphenicols

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