高效液相色谱-串联质谱法测定蜂蜜中的甲基乙二醛

Determination of methylglyoxal in honey by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  麦卢卡蜂蜜  甲基乙二醛  高效液相色谱-串联质谱法

英文关键词:Manuka honey  methylglyoxal  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种蜂蜜中甲基乙二醛的高效液相色谱-串联质谱法的测定方法。方法 采用高效液相色谱-串联质谱法测定蜂蜜中的甲基乙二醛, 蜂蜜样品直接用水提取, 2,3-二氨基萘为衍生化试剂, 常温下避光反应8 h 以上, 以0.1%甲酸水-乙腈为流动相, 色谱柱分离, 通过质谱电喷雾离子源, 正离子模式进行定性和定量分析。结果 甲基乙二醛的线性范围为0.05~1.0 μg/mL, 相关系数0.999 以上, 线性良好, 检出限为0.2 mg/kg, 定量限为0.5 mg/kg。回收率92.4%~97.5%之间, 相对标准偏差(relative standard deviation, RSD)均 小于1.3%。结论 该方法的精密度、回收率均满足要求, 适用于大批量样品的快速检测。

英文摘要:

      Objective To establish a method for determination of methylglyoxal in honey by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Methylglyoxal was determined in honey by HPLC-MS/MS. Honey samples were directly dissolved with water, and derivatizated by 2,3-diaminonaphthalene as reagent under room temperature and away from light for reaction more than 8 hours. With acetonitrile and 0.1% formic acid water as mobile phase, samples were separated by chromatographic column. Under electrospray ion source and positive ion mode, the qualitative and quantitative analysis were carried out. Results In the linear range of 0.05-1.0 μg/mL, the correlation coefficient were above 0.999, limit of detection was 0.2 mg/kg,and limit of quantitation was 0.5 mg/kg. The recoveries were 92.4%-97.5% and relative standard deviations (RSDs) were below 1.3%. Conclusion The method has high accuracy and recoveries, which meets detection requirements and is suitable for rapid detection of bulk sample.