[通过微生物筛选、高效液相色谱法和液相色谱/串联质谱法快速测定肉类中4种四环素残留量]

[Rapid determination of residues of 4 tetracyclines in meat by a microbiological screening, HPLC and LC/MS/MS].

作者信息

Kanda Maki, Kusano Tomoko, Osanai Taka, Ushiyama Keiko, Takeba Kazue, Sakamoto Miho, Hayashi Hiroshi, Igusa Kyoko, Ibe Akihiro, Nagayama Toshihiro

机构信息

Tokyo Metropolitan Institute of Public Health, Tokyo, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2008 Feb;49(1):37-44. doi: 10.3358/shokueishi.49.37.

DOI:10.3358/shokueishi.49.37

PMID:18344657

Abstract

A rapid and precise determination residues of 4 tetracyclines (TCs) (oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DOXY)) in meat was developed by employing three analyses; a microbiological screening, HPLC and LC/MS/MS. TCs were extracted with pH 4.0 McIlvaine buffer containing 0.01 mol/L EDTA from a meat sample, and then purified using a mixed mode, reversed-phase and cation-exchange cartridge. The mean recoveries (n=5) of 0.2 microg/g OTC, TC and CTC, 0.05 microg/g DOXY spiked in meat samples were 76.6-99.0% (C.V. 1.6-5.4%). In 13 meat samples in which the microbiological screening indicated the presence of TCs, CTC (9 samples) and DOXY (4 samples) were identified with HPLC and LC/MS/MS.

摘要

通过采用三种分析方法（微生物筛选、高效液相色谱法（HPLC）和液相色谱-串联质谱法（LC/MS/MS）），建立了一种快速、精确测定肉类中4种四环素（TCs）（土霉素（OTC）、四环素（TC）、金霉素（CTC）和强力霉素（DOXY））残留量的方法。用含有0.01 mol/L乙二胺四乙酸（EDTA）的pH 4.0麦氏缓冲液从肉类样品中提取四环素，然后使用混合模式、反相和阳离子交换柱进行纯化。在肉类样品中添加0.2 μg/g的OTC、TC和CTC以及0.05 μg/g的DOXY，平均回收率（n = 5）为76.6% - 99.0%（变异系数为1.6% - 5.4%）。在13份微生物筛选表明存在四环素的肉类样品中，通过HPLC和LC/MS/MS鉴定出了金霉素（9份样品）和强力霉素（4份样品）。