摘要
提出了超高效液相色谱-串联质谱法测定水产品中氯霉素和氟苯尼考含量的方法。样品粉碎后以乙酸乙酯为萃取溶剂经加速溶剂萃取仪在100℃静态萃取5min,提取液浓缩后溶于水中并用正己烷萃取净化。采用Thermo Hypersil GOLD C18色谱柱分离,以甲醇和水按不同比例混合为流动相作梯度淋洗。质谱测定中采用电喷雾负离子扫描、选择反应监测模式进行测定。氯霉素和氟苯尼考在0.02～10μg·kg-1范围内呈线性,检出限(3S/N)为0.02μg·kg-1,测定下限(10S/N)为0.05μg·kg-1。以空白水产品为基体,在4个浓度水平进行加标回收试验,氯霉素和氟苯尼考的回收率在90.2%～109%之间,相对标准偏差(n=6)在1.8%～8.5%,
A method of UHPLC MS/MS for the simultaneous determination of chloramphenicol and florfenicol in aquatic products was proposed. The sample was crushed and extracted with ethyl acetate under static condition at 100℃ for 5 min by accelerated solvent extraction （ASE）. The extract was concentrated, dissolved in water and purified by extraction with n hexane. Thermo Hypersil GOLD C18 chromatographic column was used as stationary phase, and a mixture of methanol and water in different ratios was used as mobile phase in gradient elution. The ionization modes of ES1 with SRM mode of detection were adopted in MS/MS determination. Linearity ranges of chloramphenicol and florfenicol were kept same from 0. 02 to 10 μg ·kg -1 with detection limits （3S/N） of 0. 02 μg ·kg -1 and lower limits of determination （10S/N） of 0. 05 μg ·kg -1 Tests for recovery were made by addition of standards of chloramphenicol and florfenicol at 4 different concentration levels to blank aquatic product samples, values of recovery found were in the range of 90. 2%-109% with values of RSD＇s （n=6） in the range from 1.8 % to 8. 5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2012年第11期1353-1356,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
江苏省基础设施建设计划(BM2008258)
江苏省水产三项工程(PJ2010-52)
