[经9-芴甲氧羰基（FMOC）衍生化及高效液相色谱分离后荧光法测定动物源性食品中的红霉素残留量]

[Fluorimetric determination of erythromycin residues in foods of animal origin after derivatization with FMOC and HPLC separation].

作者信息

Zierfels G, Petz M

机构信息

Universität GH Wuppertal, Fachbereich 9 (Chemie, Lebensmittelchemie), Wuppertal, Germany.

出版信息

Z Lebensm Unters Forsch. 1994 Apr;198(4):307-12. doi: 10.1007/BF01193180.

DOI:10.1007/BF01193180

PMID:8197827

Abstract

A high-performance liquid chromatographic (HPLC) method for the determination of the macrolide antibiotic erythromycin in eggs, milk, swine muscle, kidney and liver was developed. The drug was extracted from the matrix with acetonitrile. The raw extract was purified by liquid-liquid partitioning and fractionation by reversed-phase HPLC for additional cleanup. Erythromycin was reacted in a pre-column procedure with 9-fluorenylmethylchloroformate (FMOC) to enable fluorimetric detection (excitation 255 nm, emission 315 nm) after isocratic separation on an analytical RP-18 HPLC column. Mean recoveries ranged from 99% at fortification levels of 0.03 mg/kg in egg to 38% at 0.06 mg/kg in liver. With the exception of liver all detection limits were below 0.01 mg/kg and precision for all other matrices and tested concentrations (0.015-0.09 mg/kg) better than 20% (coefficient of variation).

摘要

建立了一种高效液相色谱（HPLC）法，用于测定鸡蛋、牛奶、猪肌肉、肾脏和肝脏中的大环内酯类抗生素红霉素。药物用乙腈从基质中提取。粗提取物通过液-液分配和反相HPLC分级纯化以进一步净化。红霉素在柱前程序中与9-芴基甲基氯甲酸酯（FMOC）反应，以便在分析型RP-18 HPLC柱上进行等度分离后进行荧光检测（激发波长255 nm，发射波长315 nm）。平均回收率范围从鸡蛋中强化水平为0.03 mg/kg时的99%到肝脏中0.06 mg/kg时的38%。除肝脏外，所有检测限均低于0.01 mg/kg，所有其他基质和测试浓度（0.015 - 0.09 mg/kg）的精密度优于20%（变异系数）。