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C18SPE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0.020μg/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。
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 G18 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 μ g/ml and the linear range was 0.01 - 25μ g/ml, and the spike recoveries at three levels of 0.02 - 5 μ g/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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2009年第14期207-209,共3页
Food Science
基金
河北省教育厅科学研究计划资助项目(2005322)
