食品科学 ›› 2013, Vol. 34 ›› Issue (10): 180-183.doi: 10.7506/spkx1002-6630-201310039

• 分析检测 • 上一篇    下一篇

高效液相色谱法同时测定鸡肉中3种四环素类抗生素残留

葛云芝,于小波,周光宏*,徐幸莲   

  1. 南京农业大学 教育部肉品加工与质量控制重点实验室,江苏 南京 2100953. 南京农业大学国家肉品质量安全控制工程技术研究中心
  • 收稿日期:2012-03-02 修回日期:2013-04-10 出版日期:2013-05-25 发布日期:2013-05-07
  • 通讯作者: 葛云芝 E-mail:2010108059@njau.edu.cn

Simultaneous Determination of 3 Tetracycline Residues in Chicken Tissues by High-Performance Liquid Chromatography

GE Yun-zhi,YU Xiao-bo,ZHOU Guang-hong*,XU Xing-lian   

  1. Key Laboratory of Meat Processing and Quality Control, Ministry of Education, Nanjing Agricultural University, Nanjing 210095, China
  • Received:2012-03-02 Revised:2013-04-10 Online:2013-05-25 Published:2013-05-07
  • Contact: Yun-zhi GE E-mail:2010108059@njau.edu.cn

摘要:

建立同时测定鸡肉组织中四环素、土霉素、金霉素3种四环素类抗生素残留的高效液相色谱分析方法。样品经柠檬酸缓冲液(pH4)、20%三氯乙酸提取后,C-18E固相萃取柱净化,用高效液相色谱C18柱分离,乙腈-甲醇-草酸作为流动相,流速为1.0mL/min,梯度洗脱,紫外检测波长为351nm,外标法峰面积定量。3种四环素类抗生素在质量浓度范围内线性良好,R2均大于0.99,鸡肉组织样品在500μg/kg添加水平的添加回收率为86.2%~89.3%,相对标准偏差为0.854%~1.213%(n=10),方法的定量限为10μg/kg。该方法灵敏度高、重复性好,适用于鸡肉组织中四环素、土霉素、金霉素残留的检测。

关键词: 鸡肉, 四环素, 土霉素, 金霉素, 高效液相色谱法

Abstract:

A simultaneous high performance liquid chromatography (HPLC) method was developed for the determination
of 3 tetracycline residues in chicken tissues. Chicken tissue samples were extracted with citrate buffer (pH 4) and 20% TCA,
and clean-up on C-18E solid phase (SPE) cartridge. Chromatographic separation was performed on a C18 column with a mobile
phase consisting of acetonitrile and methanol and oxalic acid at a flow rate of 1.0 mL/min by gradient elution. Detection
wavelength was 351 nm and external standard method was used for quantification. The calibration curves of 3 tetracyclines
exhibited good linearity with correlation coefficients of 0.99. The average recovery rate for 3 tetracyclines in chicken tissues
spiked at 500 μg/kg varied from 86.2% to 89.3%, with relative standard deviations between 0.854% and 1.213% (n = 10).
The limit of quantification was 10 μg/kg.

Key words: chicken tissue, tetracycline, oxytetracycline, chlorotetracycline, high performance liquid chromatography

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