一种快速痕量检测蜂蜜中氯霉素残留方法的研究

Study on Rapid Determination of Chloramphenicol in Honey at Trace Level

采用高效液相色谱-串联质谱联用技术(HPLC-MS/MS)建立快速痕量检测蜂蜜中氯霉素的内标(氘代氯霉素,D5-CAP)定量方法。在超声波辅助下,样品用乙酸乙酯进行碱性提取、净化后,以乙腈-水为流动相,并在电喷雾离子源负离子模式下进行多反应监测,实现对氯霉素的定性、定量分析,分析时间为8 min。在检测范围为0.1～20μg/mL内呈良好的线性关系,相关系数大于0.999 0。当添加水平分别为0.20、0.50、5.0μg时,氯霉素的加标回收率为84.0%～104.2%,相对标准偏差为1.95%～5.04%。方法检出限为0.013μg/kg,定量限为0.025μg/kg。所建立的方法快速高效,样品前处理简单,选择性好,灵敏度高,适用于蜂蜜中氯霉素残留的痕量检测。

A high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS） method was developed for the rapid and simple determination of chloramphenicol （CAP） in honey at trace level and D5-chloramphenicol （D5-CAP） as internal standard was used for quantification. With ultrasonic-assistance, Honey samples were extracted by ethyl acetate and detected by an MRM acquisition method in negative ionization mode. A mixture of acetonitrile-water as mobile phase was used. The analysis time was 8 rain. The calibration curve was linear over the range of 0.1 - 20 μg/mL and the linearity was satisfactory with a correlation coefficient〉0.999 0. In the three fortified levels （0.20, 0.50 and 5.0μg）, recoveries of CAP rautged from 84.0% to 104.2% and the mean values of relative standard deviation ranging from 1.95% to 5.04% were obtained. The detection limit was 0.0 l 3 ~tg/kg and the limit of quantitation （LOQ） was 0.025 Ixg/kg. The established method was rapid and efficient, with high selectivity and sensitivity, and the sample preparation was simple. From the above, the method was suitable for the trace detection ofchloramphenicol in honey sample.