摘要
建立了同时检测蜂胶中16种磺胺及2种林可胺类药物残留的方法,以1.0 mol/L HCl溶液为提取液,经阳离子固相萃取小柱净化富集后,高效液相色谱-串联质谱仪分析。采用Agilent Polaris C18色谱柱（100 mm×2.0 mm,5μm）,以甲醇和0.1%甲酸为流动相梯度洗脱,质谱模式为电喷雾正离子监测。该方法前处理简单,分别以13C6-磺胺二甲基嘧啶、13^C6-磺胺甲噁唑为磺胺类药物内标、以D3-林可霉素为林可胺类药物内标进行定量,磺胺和林可胺类药物的线性范围均为1.0-50μg/L,相关系数均在0.99以上,方法定量限为10.0μg/kg,在10,20和40μg/kg 3个水平做添加回收,回收率范围为69.5%-114.6%,相对标准偏差小于10%。
A method for determination of sulfanilamides and lincosamides in propolis was developed by high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with hydrochloric acid solution and then cleaned up by SPE with ion-exchange cartridges. Separations were performed on an Agilent Polaris C18 column（ 100 mm × 2. 0 mm,5 μm）. The mobile phase was methanol- 0. 1% formic acid.The isotopically labeled internal standards13^C6-Sulfamethoxazol and13^C6-Sulfamethazine were used for quantitation of sulfanilamides while D3-Lincomycin was for lincosamides. The linear ranges were 1. 0- 50 μg / L and all the correlation coefficient was above 0. 99. The limit of quantitation was 10. 0 μg / kg. The recoveries ranged from 69. 5% to 114. 6 % at the concentration levels of 10,20 and 40 μg / kg while the relative standard deviation lower than 10%.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第12期1420-1424,共5页
Chinese Journal of Analysis Laboratory
基金
国家质检总局科技项目(2012IK167)资助
关键词
液相色谱-串联质谱
蜂胶
磺胺
林可胺类
High performance liquid chromatography-tandem mass spectrometry
Propolis
Sulfanilamides
Lincosamides
