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目的建立超高效液相色谱串联三重四极杆质谱法测定蜂蜜中氯霉素残留的分析方法。方法样品经乙酸乙酯提取,过固相萃取小柱净化,用Waters BEH C_(18)柱(2.1 mm×100 mm,1.7μm)分离,流动相为0.05%氨水/乙腈梯度洗脱,内标法定量,电喷雾离子MRM(multiple reaction monitoring)模式检测。结果该方法的检出限为0.01 ng/mL,样品的定量限为0.1μg/kg,线性范围为0.01～5.0 ng/mL,平均回收率为92%～105%,相对标准偏差小于4%。结论该方法灵敏、准确、快速,能满足蜂蜜中氯霉素的监督检测。
OBJECTIVE To establish a method for the determination of chloramphenicol residues in honey by ultra performance liquid chromatography tandem triple-quadrupole mass spectrometry. Methods The samples were extracted with ethyl acetate and purified by a solid phase extraction cartridge. The residue was separated on a Waters BEH C 18 column (2.1 mm × 100 mm, 1.7 μm). The mobile phase was eluted with a 0.05% aqueous ammonia / acetonitrile gradient. The internal standard Quantitative, electrospray ion MRM (multiple reaction monitoring) mode detection. Results The limit of detection was 0.01 ng / mL. The limit of quantification was 0.1 μg / kg. The linear range was 0.01-5.0 ng / mL. The average recovery was 92% -105%. The relative standard deviation was less than 4%. Conclusion The method is sensitive, accurate and rapid, which can meet the supervision and detection of chloramphenicol in honey.