【摘要】 目的建立花粉中的糖的酰胺基亲水作用色谱柱分离的高效液相色谱-蒸发光散射检测方法,分析比较不同花粉中糖花粉中的糖分特征。方法花粉样品经40%乙腈超声提取,过Waters XBridge Amide (4. 6 mm×250 mm,3. 5μm)色谱柱,以乙腈-0. 2%三乙胺为流动相进行梯度洗脱,流速1. 0 ml/min,进样量10μl,柱温45℃,ELSD检测器漂移管温度40℃,氮气压力350 k Pa,增益6。在我国各花粉产地产品采集12种花粉样品为研究对象测定分析,统计获得中位数,比较不同花粉中的糖分特征。结果果糖、葡萄糖、蔗糖、麦芽糖得到很好的分离,线性良好,相关系数r=0. 999 7~0. 999 9。4个组分在高低水平的添加回收率(n=3)在91. 6~104%,RSD(n=3)均在4%以内。所有12种花粉样品中的果糖/葡萄糖(F/G)均大于1。蜂花粉中果糖、葡萄糖或F+G含量均大大高于松花粉,F+G的中位数:蜂花粉27. 2%,松花粉4. 28%。蔗糖含量(4. 69%)在不同类型花粉中差异较大。麦芽糖(0. 302%)在所有花粉中都是含量最微的糖分。结论本法操作简单,灵敏度高,经方法学验证结果准确可靠;本研究初步得出了各种花粉中糖分的分布特征,为花粉的评价、鉴别提供科学依据,为花粉产品的质量控制、标准修订及相关研究提供参考。更多还原

【Abstract】 Objective To establish a method by using sugar amide hydrophilic interaction chromatography with evaporative light scattering detector,and to detect the sugars content in different pollens. Methods The chromatographic separation achieved at a Waters XBridge Amide column( 4. 6 mm × 250 mm,3. 5 μm) by a gradient elution program with acetonitrile-0. 2%triethylamine as the mobile phase. The flow rate was 1. 0 m L/min,and the column temperature was 45℃. The detection performed by ELSD detector with drift tube temperature of 40℃ and gas pressure of 350 kPa. Results Fructose,glucose,sucrose and maltose were well separated. The calibration curves showed good linearity with good correlation coefficients( r = 0.9997-0. 9999). The average recoveries at high and low concentrations of 4 sugars ranged from 91. 6% to 104% with RSDs( n= 3) less than 4%. The F/G ratios of all 12 pollen samples in this study were greater than 1. The content of fructose,glucose or the F + G levels in bee pollens were much higher than those of pine pollens. The medians of F + G were 27. 2% for bee pollen,and 4. 28% for pine pollen. Sucrose content varied in different types of pollen,and Maltose content was the lowest in all pollens. Conclusion This method is simple,sensitive,accurate and reliable. The distribution characteristics of sugar in various pollen can provide a scientific basis for the evaluation and identification of pollen,so as to provide a reference for quality control,standard revision and related research of pollen products.更多还原