色谱2012，Vol.30Issue(6)：568-571,4.DOI:10.3724/SP.J.1123.2012.02003
高效液相色谱-串联质谱法检测奶中克拉维酸残留
Determination of clavulanic acid residue in milk by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
An analytical method was developed for the determination of clavulanic acid (CLAV) in milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A 2 g milk sample was deproteinized by ethanol. The supernatant was transferred into a pear-shaped bottle to be evaporated to about 0. 5 mL, and the residue was dissolved with ammonium acetate solution. The sample was determined by HPLC-MS/MS after the purification. The chromatographic separation was achieved on a Luna 5u C8column using 0. 1% formic acid in water and acetonitrile as mobile phases with gradient elution. The identification of CLAV was carried out by MS/MS equipped with electrospray ionization in negative scanning and multiple reaction monitoring (MRM) modes. Matrix-matched calibration standard was used for the quantification. The calibration curve showed perfect linear in the range of 10 -400μg/kg with the correlation coefficient of 0. 999. The limit of detection (LOD, S/N>3) was 10μg/kg in milk, and the limit of quantification (LOQ, S/N≥10) was 20μg/kg. The mean recoveries varied from 80. 00% to 91. 25% at the four spiked levels of LOQ, 1/2MRL (the maximum residue limit), MRL, and 2MRL with the relative standard deviations of 5. 60% -8. 77%. In conclusion, the established method can be applied for the determination of CLAV residues in milk.关键词
高效液相色谱-串联质谱/克拉维酸/奶Key words
high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/ clavulanic acid/ milk分类
化学化工引用本文复制引用
杨刚,黄显会,郭春娜,方秋华,贺利民..高效液相色谱-串联质谱法检测奶中克拉维酸残留[J].色谱,2012,30(6):568-571,4.基金项目
2010年农业行业标准制修订项目. （）
