超高效液相色谱串联质谱法测定龙眼干中5-羟甲基糠醛

The determination of 5-hydroxymethylfurfural in dried longan by ultra perfor⁃mance liquid chromatography-tandem mass spectrometry

目的:建立超高效液相色谱串联质谱法测定龙眼干中5-羟甲基糠醛。方法:样品采用甲醇水溶液(2:8,V:V)提取,提取液用乙酸乙酯液液萃取,乙酸乙酯层于40℃下旋转浓缩至干,用1.0mL甲醇+0.1%甲酸水(2:8,V:V)溶解残渣,样液过0.22μm滤膜后经C18柱分离,电喷雾正离子扫描模式下多反应监测方式检测,外标法定量。结果:5-羟甲基糠醛在5.0-250μg/L的浓度范围内,具有良好的线性关系,相关系数为0.9976,在龙眼干中样品添加浓度为100μg/kg、200μg/kg水平下平均回收率为95.1%-96.3%,相对标准偏差为6.1%-7.1%,检出限为2.0μg/kg,龙眼干样品实际检测中,5-羟甲基糠醛含量0.0888-16.7mg/kg。结论:该方法准确、灵敏、快速,是检测龙眼干中5-羟甲基糠醛的有效方法。

Objective:To establish a method for the determination of 5-hydroxymethylfurfural in dried longan by ultra perfor⁃mance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The samples were extracted with methanol aqueous solution(2:8,V/V),the ethyl acetate layer were concentrated to dry at 40℃after added ethyl acetate in⁃to the extracting solution.Then utilizing 1.0 mL solution containing methanol+0.1%formic acid(2:8,V:V)to dissolve the residue.The sample solution was separated by a C18 column after used of 0.22μm filter membrane.Detected by UPLC-MS/MS in the multi reaction monitoring mode with electric spray positive ion scanning,and the external standard method was used for quantification.Results:The linear correlation coefficient of method for 5-hydroxymethylfurfural is 0.9976 at range of 5.0-250μg/L,the average recovery rate of the sample at the concentration of 100μg/kg and 200μg/kg is95.1-96.3%,the relative standard deviation is 6.1-7.1%,and the limit of detection(LOD)is 2.0μg/kg.The content of 5-hydroxymethylfur⁃fural is 0.888-16.7mg/kg in real test of dry longan samples.Conclusion:This method is accurate,sensitive and rapid,which is an effective method for the determination of 5-hydroxymethylfurfural in dried longan.