【摘要】 目的建立猪肉和鱼肉中氯霉素残留的超高效液相色谱-串联质谱（UPLC-MS/MS）检测方法。方法以氘代氯霉素为内标,用含0.2%甲酸乙腈-水（80:20）提取样品中的氯霉素, Oasis PRiME HLB柱净化,采用BEH C₁₈（2.1 mm×100 mm,1.7μm）柱分离,柱温为30℃,以乙腈-0.1%甲酸的水溶液为流动相,梯度洗脱,流速为0.25 ml/min;质谱检测,ESI^-模式。结果方法线性范围为0.1μg/L～10μg/L,目标物在测定的浓度范围内,线性关系良好,相关系数>0.999 9,检出限为0.012μg/kg;用3种浓度做加标回收,回收率为83.2%～91.2%,相对标准偏差为2.94%～6.26%。结论本法快速、灵敏,操作简便,检测结果准确度高,能满足日常猪肉和鱼肉样品中的氯霉素残留的检测要求。更多还原

【Abstract】 Objective To establish a method for the determination of chloramphenicol residues in pork and fish with liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods Using deuterated chloramphenicol as the internal standard, chloramphenicol was extracted from the sample using 0.2% acetonitrile formate-water（80:20, V/V）, then purified with Oasis PRiME HLB column, and finally separated with BEH C₁₈（2.1 mm×100 mm, 1.7 μm） column when temperature was 30 ℃. Acetonitrile-0.1% formic acid aqueous solution was used as a mobile phase for gradient elution with the flow rate 0.25 ml/min. The detection was performed by using mass spectrometer and ESI^- mode. Results The linear range was within 0.1 μg/L-10 μg/L, and the target had a good linear relationship in the determined concentration range, with the correlation coefficient greater than 0.999 9. The detection limit was set as 0.012 μg/kg. Three concentrations were used for standard recovery, which was within 83.2%-91.2%, and the relative standard deviation was within 2.94%-6.26%. Conclusion This method is quick, sensitive, easy-operate, and accurate. It can be applied to the determination of chloramphenicol residue in daily pork and fish samples.更多还原