液相色谱-荧光检测法检测水产品中甲砜霉素、氟甲砜霉素及代谢物氟甲砜霉素胺残留

Determination of Thiamphenicol, Florfenicol and Florfenicol Amine Residues in Aquatic Products by HPLC with Fluorescence Detection

关键词:  液相色谱-荧光检测  甲砜霉素  氟甲砜霉素  氟甲砜霉素胺  残留  水产品

Key words:  HPLC-FLD  Thiamphenicol  Florfenicol  Florfenicol amine  Residue  Aquatic products

摘要:

建立了以带荧光检测器的液相色谱检测水产品中甲砜霉素、氟甲砜霉素与氟甲砜霉素胺残留的新方法。采用碱性乙酸乙酯-乙腈提取试样中残留的化合物，凝胶渗透色谱（GPC）净化，荧光检测器的激发与发射波长分别为225nm与295nm，可疑样品以液相色谱-质谱/质谱进行确证。在添加浓度为0.050 ～ 2.0 mg/kg时，平均回收率在86.4～96.8%之间，相对标准偏差（RSD）在5.63 ～9.71%之间（n=5）；甲砜霉素、氟甲砜霉素在0.20 ～ 5.0 mg/L范围内、氟甲砜霉素胺在0.10 ～ 5.0 mg/L范围内有良好的线性关系，甲砜霉素与氟甲砜霉素的检测限达0.020 mg/kg、氟甲砜霉素胺的检测限达0.010 mg/kg。

Abstract:

A novel procedure for the determination of thiamphenicol(TAP), florfenicol(FF) and florfenicol amine(FFA) in aquatic products, using high performance liquid chromatography (HPLC) with fluorescence detector was described. The analytes were extracted by basic ethyl acetate-acetonitril, gel permeation chromatography (GPC) was used for cleanup, excitation and emission wavelength were 225nm and 295nm for fluorescence detection.The average recoveries and relative standard deviations (RSDs) for the analysis of all samples fortified over the range of 0.050 - 2.0 mg/kg were in the range of 86.4% - 96.8% and 5.63% - 9.71%(n=5), respectively. Good linearities were obtained in the concenttration ranging from 0.20 to 5.0 mg/L for TAP and FF, and 0.10 to 5.0mg/L for FFA. The limits of detection were 0.020 mg/kg for TAP and FF, and 0.010mg/kg fro FFA.