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0.02~10 μg·kg-1范围内呈线性,检出限(3S/N)为0.02 μg·kg-1,测定下限(10S/N)为0.05 μg·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 ESI- 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%.