食品科学 ›› 2009, Vol. 30 ›› Issue (14): 207-209.doi: 10.7506/spkx1002-6630-200914042

• 分析检测 • 上一篇    下一篇

羊乳中替米考星残留的检测方法研究

王雪敏,石玉祥,李 存   

  1. 河北工程大学农学院
  • 收稿日期:2008-10-09 修回日期:2009-01-10 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 王雪敏 E-mail:xmwanghd@163.com
  • 基金资助:

    河北省教育厅科学研究计划资助项目(2005322)

HPLC Determination of Tilmicosin Residue in Goat Milk

WANG Xue-min,SHI Yu-xiang,LI Cun   

  1. College of Agriculture, Hebei University of Engineering, Handan 056021, China
  • Received:2008-10-09 Revised:2009-01-10 Online:2009-07-15 Published:2010-12-29
  • Contact: WANG Xue-min, E-mail:xmwanghd@163.com

摘要:

建立了羊乳中替米考星残留的反相高效液相色谱检测方法。羊乳按1:1(V/V)用乙腈提取,上清液以5ml/min 流速过C18 SPE 柱,采用乙腈- 水(20:80,V/V)洗涤、乙腈- 水(90:10,V/V)洗脱,并以0.1mol/L 乙酸铵- 乙腈-甲酸(60:30:10,V/V)为流动相,采用高效液相色谱仪在280nm 处使用紫外检测器检测。本法定量限(LOQ)为0.02μg/ml,平均回收率范围在90.3%~98.1% 之间,线性范围为0.01~25μg/ml,变异系数范围在4.1%~8.9% 之间。本法可满足残留分析的要求,为羊乳中替米考星的残留分析提供了可靠的检测方法。

关键词: 羊乳, 替米考星, 高效液相色谱, 残留检测

Abstract:

A reverse phase HPLC method was developed for the determination of tilmicosin residue in goat milk. Samples were extracted using methanol, and cleaned-up using SPE on a C18 cartridge with a mixture of acetonitrile and water (90:10, V/V) as the eluent [the washing with a mixture of acetonitrile and water (20:80, V/V) was carried out prior to elution]. The analysis was performed on a Symmetry column with a mobile phase composed of 0.1 mol/L ammonium acetate (adjusted to pH 5.0 with formic acid), acetonitrile and methanol (60:30:10, V/V) using a UV detector set at 280nm. The limit of quantification was 0.020 μg/ml and the linear range was 0.01-25 μg/ml, and the spike recoveries at three levels of 0.02-5 μg/ml were in the range of 90.3%-98.1% with a coefficients of variation ranging 4.1%-8.9%. The method can meet the requirement for tilmicosin residue analysis.

Key words: goat milk, tilmicosin, HPLC, residue determination

中图分类号: