固相萃取-高效液相色谱法测定椴树蜜特征成分椴树素

Determination of the unique ingredient lindenin in linden honey by solid phase extraction and high performance liquid chromatography

目的建立固相萃取-高效液相色谱法测定椴树蜜特征成分椴树素含量.方法蜂蜜经水溶解后,通过Strata-X-A固相萃取柱对椴树素富集净化,采用Mightysil RP-18色谱柱进行分离,以1%(V/V)乙酸水溶液和甲醇为流动相进行梯度洗脱,外标法定量.对固相萃取柱规格、样品溶液pH、淋洗条件和洗脱条件等实验条件进行选择和优化.结果在优化的实验条件下,椴树素在1~200 mg/L范围内呈良好线性关系,相关系数为0.9998,检出限为0.03 mg/kg,定量限为0.10 mg/kg;在5个添加水平下,椴树素的回收率为84.03%~96.65%,精密度为0.95%~2.61%(n=6).结论本方法操作简便、灵敏度高、准确性好,适用于椴树素的定量检测.

Objective To establish a method for the determination of the unique ingredient lindenin in linden honey by solid phase extraction and high performance liquid chromatography.Methods Honey sample was dissolved in water,enriched and purified by a Strata-X-A solid phase extraction column,separated on a Mightysil RP-18 column by a gradient elution with 1%(V/V)acetic acid water and methanol as mobile phases,and quantified by an external standard method.The experimental conditions such as the specification of the solid phase extraction column,the pH of the sample solution,the washing and the elution parameters were selected and optimized.Results Under the optimized experimental conditions,lindenin showed a good linear relationship in the range of 1-200 mg/L,the correlation coefficient was 0.9998,and the limit of detection and quantification for lindenin were 0.03 mg/kg and 0.10 mg/kg,respectively.At 5 levels of addition,the recoveries of lindenin ranged from 84.03%to 96.65%,with relative standard deviations between 0.95%and 2.61%(n=6).Conclusion The proposed method is simple to operate,highly sensitive and accurate,and is applicable for the quantitative detection of lindenin and further used for the authenticity assessement of linden honey.