›› 2011, Vol. 38 ›› Issue (3): 163-166.

• 疾病防治 • 上一篇    下一篇

高效液相色谱荧光检测法检测鸡肉中甲砜霉素残留

谢恺舟1,徐东1,陈书琴1,谢星2,黄玉萍1,贾龙飞1,郭辉生1,王金玉1   

  1. (1.扬州大学动物科学与技术学院,江苏省动物遗传繁育与分子设计重点实验室,江苏扬州 225009; 2.扬州大学兽医学院,江苏扬州 225009)
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2011-03-20 发布日期:2011-03-20

Determination of Residues of Thiamphenicol in Chicken Muscle by HPLC with Fluorescence Detection

XIE Kai-zhou1,XU Dong1,CHEN Shu-qin1,XIE Xing2,HUANG Yu-ping1,JIA Long-fei1,GUO Hui-sheng1,WANG Jin-yu1   

  1. (1.Key Laboratory for Animal Genetic,Breeding,Reproduction and Molecular Design of Jiangsu Province,College of Animal Science and Technology,Yangzhou University,Yangzhou 225009,China;2.College of Veterinary Medicine,Yangzhou University,Yangzhou 225009,China)
  • Received:1900-01-01 Revised:1900-01-01 Online:2011-03-20 Published:2011-03-20

摘要: 研究建立了用高效液相色谱荧光法检测鸡肉中甲砜霉素残留的方法。鸡肉经丙酮、二氯甲烷提取,饱和正己烷脱脂,氮吹仪吹干浓缩后,以乙腈―磷酸二氢钠溶液(0.01 mol/L,含0.005 mol/L十二烷基硫酸钠和0.1%三乙胺)(32∶68,V/V)为流动相,流速为1.0 mL/min,荧光检测激发波长为225 nm,发射波长为290 nm。甲砜霉素在0.01~1.75 mg/L浓度范围内,本方法线性关系良好,相关系数为0.9991。当甲砜霉素添加水平为5~500 μg/kg时,该方法平均回收率为79.49%~89.71%,相对标准偏差为4.96%~9.61%;日内相对标准偏差为5.68%~7.47%;日间相对标准偏差为8.89%~11.32%。甲砜霉素检测限为1.5 μg/kg(S/N=3),定量限5 μg/kg(S/N=10)。所建立的方法简便、快速、灵敏度高,适用于鸡肉中甲砜霉素残留的高灵敏度检测。

关键词: 高效液相色谱; 荧光检测法; 甲砜霉素; 鸡肉; 残留

Abstract: A high performance liquid chromatography with fluorescence detection(HPLC-FLD) method was built for determination of residues of thiamphenicol(TAP) in chicken muscle. TAP was extracted with acetone and dichloromethane from chicken muscle. Extract solution was degreased with n-hexane and evaporated with nitrogen evaporator,the mobile phase was acetonitrile-sodium dihydrogen phosphate solution(0.01 mol/L,containing 0.005 mol/L SDS and 0.1% triethylamine)(32∶68),the flow rate was 1.0 mL/min. The fluorescence detection was with an excitation wavelength of 225 nm and an emission wavelength of 290 nm. The data showed that the linear relationship of TAP was nice (r=0.9991) in 0.01 mg/L to 1.75 mg/L concentration range. At spiked level 5 to 500 μg/kg for TAP,the average recovery ranged from 79.49% to 89.71%,relative standard deviation(RSD) ranged from 4.96% to 9.61%,the within-day RSD ranged from 5.68% to 7.47%,the between day RSD ranged from 8.89% to 11.32%. The lowest detection limit of TAP was 1.5 μg/kg(S/N=3) and the lowest quantitative limit of TAP was 5 μg/kg (S/N=10). This HPLC-FLD method is simple,rapid,high sensitivity and suitable for high sensitivity determination of TAP in chicken muscle.

Key words: high performance liquid chromatography(HPLC); fluorescence detection; thiamphenicol(TAP); chicken muscle; residues

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