超高效合相色谱-蒸发光散射检测法测定蜂蜜中4种单、双糖的含量

摘要

采用超高效合相色谱-蒸发光散射检测( UPC2-ELSD)技术,建立了测定蜂蜜中4种单、双糖含量的方法。其中单糖为果糖和葡萄糖,双糖为蔗糖和麦芽糖。以ACQUITY UPC2BEH(100 mm×3.0 mm,1.7μm)为色谱柱,超临界CO2和甲醇(含0.2%氨水, V/V)作为流动相,流速为1.0 mL/min,柱温为50℃,ELS为检测器,漂移管温度为50℃,N2压力为260.7 kPa(30 psi)。研究表明,4种单、双糖化合物在线性范围内线性关系良好,线性相关系数(R)均大于0.9983；目标物的检出限(S/N≥3)为2.0~4.7 mg/L；3个加标水平下的回收率为86.6%~103.8%,相对标准偏差为1.8%~4.3%。此方法简单、快速、分离效果好、分析成本低,是一种测定蜂蜜样品中单、双糖的优良方法,且检测结果与国家标准方法保持一致。%A method for determination of four monosaccharides and disaccharides in honey was established by ultra performance convergence chromatography coupled with evaporative light scattering detector ( ELSD) . The monosaccharides are fructose and glucose, and the disaccharides are sucrose and maltose. The chromatographic separation was conducted on an ACQUITY UPC2 BEH column (100 mmí3. 0 mm, 1. 7 μm) using carbon dioxide and methanol ( containing 0. 2% ammonium hydroxide, V/V) as gradient elution. The flow rate was 1 . 0 mL/min with column temperature at 50℃. The drift tube temperature of the ELSD was set at 50℃ and the pressure of N2 was set at 260. 7 kPa. It was found that the reasonable linearity was achieved for monosaccharides and disaccharides with correlation coefficients not less than 0 . 9983 . The limits of detection (S/N≥3) of the four saccharides were 2. 0-4. 7 mg/L. The recoveries for the four monosaccharides and disaccharides at three spiked levels were 86 . 6%-103 . 8% with relative standard deviations of 1 . 8%-4 . 3%. This method can be regarded as an excellent method for the determination of monosaccharides and disaccharides in honey samples, with the advantages of simplicity, rapidness, good separability and low cost. The detection result was consistent with that of national standard method.