采用高效液相色谱- DAD检测法测定蜂蜜中抗生素残留

Bouchra Rachi̇d, A. Jaber, Edmond Cheble
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摘要

秘密地,消费者可能会接触到蜂蜜中的抗生素(ATB)残留,这可能会造成健康问题。本文首次建立了氟苯尼考(FF)、青霉素G (PG)和四环素的同时测定方法。采用高效液相色谱(HPLC)耦合二极管阵列检测器(DAD),建立并优化了多残留检测方法。这些ATBs在C18分析柱上经过净化后的固相萃取(SPE)分离。首次完善了色谱条件。在方法验证过程后,采用该方法对4种黎巴嫩蜂蜜样品中的ATB残留进行了评价。用80%磷酸二氢钾水溶液和20%乙腈的混合物等密度洗脱,在不到15分钟的时间内分离ATBs。TC、FF、PG的紫外检测波长分别为350 nm、224 nm和230 nm,在0.7 ~ 17.5 mg浓度范围内呈线性关系(R2≥0.996)。三种化合物的千克1。日内和日间的精密度(RSD)均≤15%。该方法随后成功地应用于分析黎巴嫩养蜂蜂蜜样品中检测到的ATB残留。所描述的方法可能是对黎巴嫩生产的蜂蜜样品进行全面调查的宝贵工具,特别是在缺乏认真的国家监督的情况下。
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Multiresidue chromatographic method for the determination of antibiotic residues in honey by high-performance liquid chromatography with DAD detection
Clandestinely, consumers may be exposed to antibiotic (ATB) residues in honey, which could pose a health concern. For the first time, the simultaneous determination of Florfenicol (FF), Penicillin G (PG), and Tetracycline is described in this paper. The multiresidual method was developed and optimized using high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD). These ATBs were separated on a C18 analytical column after a cleanup process followed by solid-phase extraction (SPE). For the first time, the chromatographic conditions were perfected. After the method validation process, the method was used to assess ATB residues in four Lebanese honey samples. ATBs were separated in less than 15 min with an isocratic elution using a mixture of 80 % potassium dihydrogen phosphate aqueous solution, and 20 % acetonitrile. The UV detection was performed at 350 nm for TC, 224 nm for FF, and 230 nm for PG. The proposed method was linear (R2 ≥ 0.996) within the concentration ranges of 0.7-17.5 mg.Kg 1 for the three compounds. Both intra- and inter-day precision, expressed as RSD, were ≤15 %. The method was subsequently successfully applied to analyze examined ATB residues in honey samples collected from Lebanese beekeeping. The method described could be a valuable tool to conduct a comprehensive survey of honey samples produced in Lebanon, especially in the lack of serious national oversight.
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