高效液相色谱串联质谱法测定红糖中5-羟甲基糠醛

建立了红糖中5-羟甲基糠醛的高效液相色谱串联质谱检测方法。红糖样品经甲醇-水(V/V=5/95)充分溶解提取,经HLB柱富集净化,氮吹干洗脱液,用乙腈-水(V/V=1/9)复溶,供高效液相色谱串联质谱仪检测。以甲醇和水为流动相梯度洗脱,用Phenomenex Luma Omega C18柱(1.6μm,100 mm×2.1 mm)分离,电喷雾正离子模式(ESI+)扫描,多反应监测模式(MRM)采集数据,外标法定量。该方法在0.5~50.0μg/L范围内线性关系良好(r²=0.9999),检出限为0.44μg/kg,定量限为1.47μg/kg。在2.0、5.0、10.0μg/kg的加标水平下,5-羟甲基糠醛的平均回收率为86.3%~97.8%,相对标准偏差为2.1%~5.0%(n=6)。本方法操作简单、灵敏度高、准确度和净化效果好,适用于红糖中5-羟甲基糠醛的残留量测定。

Determination of 5-hydroxymethylfurfural in Brown Sugar by HPLC-MS/MS

A method for the detection of 5-hydroxymethylfurfural in brown sugar by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established.The brown sugar sample was fully dissolved and extracted with methanol-water solution(V/V=5/95),enriched and purified by the HLB column.The filtrate was concentrated by nitrogen,and then reconstituted with acetonitrile-water solution(V/V=1/9).Chromatographic separation was performed on a Phenomenex Luma Omega C18 column(1.6μm,100 mm×2.1 mm)with methanol and water as mobile phase,gradient elution was employed,5-hydroxymethylfurfural was monitored in the multiple reaction monitoring(MRM)mode with positive electrospray ionization(ESI+)and quantified by the external standard method.In this method,good linearity was obtained in the range of 0.5~50.0μg/L(r²=0.9999),the average recoveries of 5-hydroxymethylfurfural at three levels of 2.0,5.0,and 10.0μg/kg were from 86.3%to 97.8%with the RSDs of 2.1%~5.0%(n=6).This method was easily and characterized with acceptable sensitivity and accuracy to be suitable for the determination of 5-hydroxymethyl furfural in brown sugar.