摘要
建立了检测鸡的皮和脂肪中抗球虫类药物的超高效液相色谱-串联质谱分析方法.样品采用甲醇、乙腈、乙酸（4∶ 1∶0.05; V/V）混合溶液提取,提取液经Sep-Pak tC18固相萃取柱富集净化,在电喷雾正离子模式下,以多反应监测模式采集数据,进行定性与定量分析.结果表明,常山酮和氯苯胍的检出限均为7.0 μg/kg,定量限为20μg/kg;盐霉素、莫能菌素、甲基盐霉素、马杜霉素和拉沙洛菌素的检出限均为5.0 μg/kg,定量限为15.0 μg/kg.本方法在15 ～ 200 μg/kg添加浓度范围内的回收率为75％～110％,日内相对标准偏差≤12.8％,日间相对标准偏差≤13.4％.
A method based on ultra performance liquid chromatography-tandem mass spectrometry （UPLC- MS/MS） has been proposed for the determination of coccidiostat residues in chicken skin and fat. The sample was extracted with the combination of methanol, acetonitrile, and acetic acid, and cleaned-up by Sep-Pak tC18 solid phase extraction cartridge. Data acquisition under positive electrospray mode was performed by applying multiple reaction monitoring for both identification and quantification. The limits of detection and quantification for halofuginone and robenidine were 7 μg/kg and 20 μg/kg, respectively. The limit of detection of salinomycin, monensin, narasin, maduramicin, and lasalocid was 5 μg/kg, and limit of quantification was 15 p,g/kg. The recovery was 75% to 110% in the spiked concentration range from 15 μg/kg to 200 μg/kg, with intra-day precision lower than 12.8% , and inter-day precision lower than 13.4%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第3期409-414,共6页
Chinese Journal of Analytical Chemistry
基金
中央高校基本科研业务资金(No.2013QJ044)资助项目
关键词
超高效液相色谱
串联质谱
抗球虫药
残留
Ultra performance liquid chromatography
Tandem mass spectrometry
Coccidiostats
Residue
