UPC^2-MS法快速检测蜂蜜中的果糖、葡萄糖、蔗糖和麦芽糖

Fast determination of fructose,glucose,sucrose,maltose in honey by ultra-performance convergence chromatography-mass spectrometry

建立了蜂蜜中果糖、葡萄糖、蔗糖和麦芽糖的超高效合相色谱-质谱(UPC2-MS)快速检测的方法。样品先用少量的水溶解,再用正己烷/异丙醇(1:1,V/V)溶解,经ACQUITY UPC2BEH(100 mm×3.0 mm,1.7μm)色谱柱分离,以超临界CO2-甲醇(含0.1%NH3·H2O,V/V)为流动相进行梯度洗脱,流速为1.8 m L/min,通过质谱检测器在负离子电喷雾模式下对目标化合物进行分析,外标法定量。检测结果表明:果糖、葡萄糖、蔗糖和麦芽糖在2~150 mg/L范围线性关系良好,R2>0.9990,定量限(LOQ,S/N≥10)为0.22~0.42 mg/L,高、中、低3个浓度水平的加标平均回收率在90.0%~107.5%范围,相对标准偏差(RSD,n=6)均小于4.0%。该方法简单快速,分离效果好,为蜂蜜中果糖、葡萄糖、蔗糖和麦芽糖的分离测定提供了新的色谱技术平台。

An ultra-performance convergence chromatography-mass spectrometry（ UPC2-MS） method was developed for the determination of fructose, glucose, sucrose and maltose in honey. The chromatographic separation was performed on the ACQUITY UPC2 BEH column（ 100 mm × 3. 0 mm,1. 7 μm） using the mobile phases of carbon dioxide and methanol（ containing 0. 1% ammonium hydroxide,V/V） solution with gradient elution. The separated compounds were detected by MS detector in negative electrospray ionization（ ESI-） and quantified by external standard method. The results showed that the reasonable linearity was achieved in the range of 2 - 150 mg/L for 4 compounds with correlation coefficients not less than 0. 9990. The limits of quantification（ LOQs,S/N ≥ 10） of 4compounds were 0. 22 - 0. 42 mg/L. The recoveries for 4 compounds at 3 spiked levels were in the range of 90. 0% - 107. 5%,with values of the relative standard deviations（ RSDs,n = 6） were less than 4. 0%.This method is accurate, rapid and good separation, which can provide a new chromatographic technology platform for the detection of fructose,glucose,sucrose and maltose in honey.