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

作　　者：徐丽[1] 李宗芮[1] 张帅[1] 孟慧琴[1] XU Li;LI Zong-Rui;ZHANG Shuai;MENG Hui-Qin(Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266001, China)

机构地区：[1]山东出入境检验检疫局,青岛266001

出　　处：《食品安全质量检测学报》2018年第7期1700-1705,共6页Journal of Food Safety and Quality

基　　金：山东出入境检验检疫局科技计划项目(SK201603)~~

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0.05~1.0μg/m L,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。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/m L, 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.

关 键 词：麦卢卡蜂蜜 甲基乙二醛 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] S896.1[理学—化学]