| 加速溶剂萃取/超高效液相色谱-荧光法检测猪肉中氟苯尼考和氟苯尼考胺残留 |
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| 引用本文： | 刁志祥,张培杨,王旭堂,谢恺舟,王波,赵霞,郭亚文,张跟喜,张涛,戴国俊,刘学忠.加速溶剂萃取/超高效液相色谱-荧光法检测猪肉中氟苯尼考和氟苯尼考胺残留[J].中国畜牧兽医,2019,46(9):2753-2759. |
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| 作者姓名： | 刁志祥 张培杨 王旭堂 谢恺舟 王波 赵霞 郭亚文 张跟喜 张涛 戴国俊 刘学忠 |
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| 作者单位： | 1. 扬州大学动物科学与技术学院, 扬州 225009;2. 教育部农业与农产品安全国际合作联合实验室, 扬州 225009;3. 扬州大学兽医学院, 扬州 225009 |
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| 基金项目： | 国家现代农业产业技术体系项目（CARS-41-G23）；扬州大学"高端人才支持计划"项目（201801）；江苏省农业科技自主创新基金项目（CX（18）3022） |
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| 摘 要： | 为给动物源性食品中同时检测氟苯尼考（FF）及其主要代谢产物氟苯尼考胺（FFA）的残留提供新的安全可靠的方法，本研究建立了猪肉中FF及FFA残留检测的加速溶剂萃取/超高效液相色谱-荧光检测（ASE/UPLC-FLD）法。试验采用乙酸乙酯：氨水（98：2，V/V）为提取剂，样品经加速溶剂萃取后浓缩，用乙酸乙酯饱和正己烷除脂，再经浓缩复溶后进行UPLC-FLD检测。结果表明，FF及其代谢产物FFA在添加浓度为9.8~400和3.2~400 μg/kg的范围内线性关系良好，相关系数（R2）分别为0.9993和0.9999。FF的检测限（LOD）和定量限（LOQ）分别为3.3和9.8 μg/kg；FFA的LOD和LOQ分别为1.2和3.2 μg/kg。样品在LOQ、0.5 MRL、1.0 MRL和2.0 MRL加标水平下的平均回收率为82.92%~96.72%，相对标准偏差（RSD）低于3.11%。综上所述，加速溶剂萃取（ASE）方法省时、环保、提取效率高，超高效液相色谱-荧光检测（UPLC-FLD）检测方法高效、灵敏、回收率高，是符合检测标准的新方法。
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| 关 键 词： | 猪肉 氟苯尼考(FF) 氟苯尼考胺(FFA) 残留 加速溶剂萃取(ASE) 超高效液相色谱-荧光检测(UPLC-FLD) |
| 收稿时间： | 2019-04-02 |
Determination of Florfenicol and Florfenicol Amine Residues in Pork by Accelerated Solvent Extraction/Ultra-high Performance Liquid Chromatography-fluorescence |
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| DIAO Zhixiang,ZHANG Peiyang,WANG Xutang,XIE Kaizhou,WANG Bo,ZHAO Xia,GUO Yawen,ZHANG Genxi,ZHANG Tao,DAI Guojun,LIU Xuezhong.Determination of Florfenicol and Florfenicol Amine Residues in Pork by Accelerated Solvent Extraction/Ultra-high Performance Liquid Chromatography-fluorescence[J].China Animal Husbandry & Veterinary Medicine,2019,46(9):2753-2759. |
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| Authors: | DIAO Zhixiang ZHANG Peiyang WANG Xutang XIE Kaizhou WANG Bo ZHAO Xia GUO Yawen ZHANG Genxi ZHANG Tao DAI Guojun LIU Xuezhong |
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| Institution: | 1. College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China;2. Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China;3. College of Veterinary Medicine, Yangzhou University, Yangzhou 225009, China |
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| Abstract: | In order to provide a new safe and reliable method for simultaneous detection of florfenicol (FF) and its metabolite florfenicol amine (FFA) residues in animal-derived foods,this study established an accelerated solvent extraction/ultra-high performance liquid chromatography-fluorescence detector (ASE/UPLC-FLD) method for the determination of FF and FFA in pork.Samples were concentrated after accelerated solvent extraction,fat was removed by n-hexane saturated with ethylacetate,then concentrated and re-dissolved before analysis in UPLC-FLD system.The results showed that FF and its metabolite FFA had a good linear relationship in the range of 9.8 to 400 and 3.2 to 400 μg/kg,respectively,and the coefficient of determination (R2) were 0.9993 and 0.9999,respectively.The limit of detection (LOD) and the limit of quantification (LOQ) of FF were 3.3 and 9.8 μg/kg,for FFA were 1.2 and 3.2 μg/kg,respectively.The average recoveries of the samples at LOQ,0.5MRL,1.0MRL and 2.0MRL spiked levels ranged from 82.92% to 96.72%,and the relative standard deviations were below 3.11%.In summary,the ASE extraction method had many advantages such as high extraction efficiency,time saving,environmental protection and so on.The UPLC-FLD method had high efficiency,sensitivity and recovery,and it provided a new method for simultaneous determination of FF and FFA residues in animal-derived food and it was a new method fitting on meets testing standards. |
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| Keywords: | pork FF FFA residue ASE UPLC-FLD |
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