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首页> 外文期刊>Journal of liquid chromatography and related technologies >Development and validation of an HPLC method for the simultaneous determination of ten sulfonamide residues in whole egg according to 2002/657/EC
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Development and validation of an HPLC method for the simultaneous determination of ten sulfonamide residues in whole egg according to 2002/657/EC

机译:根据2002/657 / EC开发并验证同时测定全蛋中十种磺酰胺残留的HPLC方法

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摘要

An HPLC method for the determination of ten sulfonamides in egg is described herein. The separation was achieved on an analytical column Kromasil, C 18 5μm, 250 × 4 mm operated at ambient temperature. The mobile phase, a mixture of 0.1% formic acid as solvent A, acetonitrile as solvent B, and methanol as solvent C was delivered to the analytical column under a gradient program. PDA detection was performed for detection and confirmation of separated analytes with monitoring at 265 nm. The examined sulfonamides were extracted from whole egg, with ethyl acetate. The method was validated according to the Decision 2002/657/EC, determining selectivity, stability, decision limit, detection capability, accuracy, precision, and linearity. Overall recoveries ranged from 92.0-113.7%. All RSD values were lower than 10%. The decision limits CCa ranged from 101.74 to108.42μg/kg, while detection capability CCb ranged from 106.84 to 119.01 mu;g/kg.
机译:本文描述了测定鸡蛋中十种磺酰胺的HPLC方法。分离是在环境温度下运行的分析柱Kromasil,C 185μm,250×4 mm上完成的。在梯度程序下,将流动相(0.1%的甲酸作为溶剂A,乙腈作为溶剂B和甲醇作为溶剂C)的混合物输送至分析柱。进行PDA检测以检测和确认分离的分析物,并在265 nm处进行监测。用乙酸乙酯从整个鸡蛋中提取所检查的磺酰胺。该方法已根据2002/657 / EC决定进行了验证,确定了选择性,稳定性,决定极限,检测能力,准确性,精密度和线性。总体回收率为92.0-113.7%。所有RSD值均低于10%。判定极限CCa范围为101.74至108.42μg/ kg,而检测能力CCb范围为106.84至119.01μg/ kg。

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