超高效液相色谱-高分辨质谱法测定蜂蜜中的3种马桑内酯

建立了采用超高效液相色谱-高分辨质谱测定蜂蜜中3种马桑内酯残留的方法。样品采用0.2 mol/L磷酸盐缓冲溶液(pH=7.5)提取,经Waters HLB小柱净化,以Phenomenex C18色谱柱进行色谱分离,通过高分辨质谱t-MS²负离子扫描模式进行定性和定量分析。结果表明3种目标化合物的检出限(LOD)均为0.05 mg/kg,定量限(LOQ)均为0.1 mg/kg。空白蜂蜜样品在0.1~0.5 mg/kg范围内的3个加标水平的平均回收率为86.3%~95.6%,相对标准偏差为3.0%~8.4%。应用该方法对从新西兰进口的麦卢卡蜂蜜进行检测,检出一份样品含羟基马桑毒素0.3 mg/kg。该方法适用于蜂蜜中马桑内酯残留的检测。

Determination of three coriaria lactones in honey by ultra high performance liquid chromatography-high resolution mass spectrometry

A method for the determination of three coriaria lactone residues in honey was developed using ultra high performance liquid chromatography-high resolution mass spectrometry. The honey samples were extracted with 0.2 mol/L phosphate buffer solution (pH=7.5), and the extracts were cleaned up with Waters HLB solid phase extraction cartridges. The extracted components were separated on a Phenomenex C18 column by gradient elution. The qualitative and quantitative analyses were operated under t-MS² by high resolution mass spectrometry. The results showed that the limits of detection and quantification for the three coriaria lactones in a spiked blank honey were 0.05 mg/kg and 0.1 mg/kg, respectively. The recoveries of the three coriaria lactones spiked in blank honey samples at the levels of 0.1 to 0.5 mg/kg were 86.3%-95.6% with the RSDs of 3.0%-8.4%. The method was applied for the determination of the manuka honey from New Zealand, and tutin was detected in one of the samples. The results showed that the method is suitable for the determination of the three coriaria lactone residues in honey.