Abstract A high-performance liquid chromatography – fluorescence detection (HPLC-FLD) method was established for the determination of piperazine residues in whole eggs, albumen, and yolk employing pre-column derivatization with dansyl chloride. The egg samples were treated by accelerated solvent extraction (ASE) and the analytes purified by solid phase extraction (SPE). Acetonitrile/ultrapure water was used as the mobile phase for gradient elution. The linear dynamic range was from 6.80 to 200.0 µg/kg for whole eggs, 7.50 to 200.0 µg/kg for albumen, and 6.50 to 200.0 µg/kg for yolk with coefficients of determination (R2) greater than or equal to 0.9992. The average recoveries of piperazine from egg samples were from 72.86 to 89.26% when the concentrations were equal to the limit of quantification, 0.5 times the maximum residue limit, equal to the maximum residue limit, and twice the maximum residue limits. The relative standard deviations were between 1.73 and 4.99%. The limits of detection of piperazine in eggs were from 1.92 to 2.50 µg/kg, and the limits of quantification were between 6.50 and 7.50 µg/kg. The method meets the requirements of the European Union, the Ministry of Agriculture of the People’s Republic of China and the U.S. Food and Drug Administration (FDA) for the determination of veterinary drug residues. The validated HPLC-FLD method was successfully applied to the determination of piperazine residues in 50 eggs purchased from local supermarkets.

中文翻译：

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使用加速溶剂萃取 (ASE) 和固相萃取 (SPE) 结合高效液相色谱法测定鸡蛋中的哌嗪 - 荧光检测 (HPLC-FLD) 和使用丹磺酰氯的柱前衍生化

摘要 建立了高效液相色谱-荧光检测（HPLC-FLD）方法，采用丹磺酰氯柱前衍生法测定全蛋、蛋白和蛋黄中哌嗪残留量。鸡蛋样品通过加速溶剂萃取 (ASE) 进行处理，分析物通过固相萃取 (SPE) 进行纯化。乙腈/超纯水用作梯度洗脱的流动相。全蛋的线性动态范围为 6.80 至 200.0 µg/kg，蛋白为 7.50 至 200.0 µg/kg，蛋黄为 6.50 至 200.0 µg/kg，决定系数 (R2) 大于或等于 0.9992。当浓度等于定量限，即最大残留限的 0.5 倍时，鸡蛋样品中哌嗪的平均回收率为 72.86% 至 89.26%，等于最大残留限量，两倍于最大残留限量。相对标准偏差介于 1.73 和 4.99% 之间。鸡蛋中哌嗪的检出限为1.92～2.50 µg/kg，定量限为6.50～7.50 µg/kg。该方法符合欧盟、中华人民共和国农业部和美国食品药品监督管理局（FDA）对兽药残留量测定的要求。经验证的 HPLC-FLD 方法成功应用于从当地超市购买的 50 个鸡蛋中哌嗪残留量的测定。定量限在 6.50 和 7.50 µg/kg 之间。该方法符合欧盟、中华人民共和国农业部和美国食品药品监督管理局（FDA）对兽药残留量测定的要求。经验证的 HPLC-FLD 方法成功应用于从当地超市购买的 50 个鸡蛋中哌嗪残留量的测定。定量限在 6.50 和 7.50 µg/kg 之间。该方法符合欧盟、中华人民共和国农业部和美国食品药品监督管理局（FDA）对兽药残留量测定的要求。经验证的 HPLC-FLD 方法成功应用于从当地超市购买的 50 个鸡蛋中哌嗪残留量的测定。