直接溶剂萃取/高压液相色谱检测杏中的β-胡萝卜素

Determination of β-carotene in apricots by direct solvent extraction and high pressure liquid chromatography

目的：建立快速测定杏中β-胡萝卜素的分析方法。方法应用直接溶剂萃取/高压液相色谱法测定三种杏中β-胡萝卜素含量。5 g杏与30 mL蒸馏水混匀,再滤去水分,加入100 mL石油醚：2,6-二叔丁基-4-甲基苯酚(2,6-di-tert-butyl-4-methylphenol, BHT)(9.9∶0.1, v/v),搅拌提取1 min,提取液过滤转移至分液漏斗,提取重复3次,将提取液中的有机相旋转蒸干,用流动相乙腈：二氯甲烷：甲醇(7∶2∶1, v/v/v)清洗烧瓶并收集,浓缩至1 mL,用0.45μm微孔滤膜过滤后取20μL进样。结果该方法检出限为0.088 mg/kg,定量限为0.23 mg/kg。β-胡萝卜素在1~50 mg/L内线性关系良好(R2＝0.9996),平均加标回收率为95.59%。样品前处理仅需20~25 min。采用该方法对三种北方杏中的β-胡萝卜素进行检测,黄杏中β-胡萝卜素含量较高。结论该方法简便、快捷、准确,适用于杏中β-胡萝卜素的快速检测。

Objective To establish a rapid determination method of β-carotene in the apricot. Methods A high pressure liquid chromatography (HPLC) method was developed for determining β-carotene in three apricots. About 5 g of apricots was homogenized with 30 mL distilled water, then filtered the water and blended with 100 mL petroleum: 2, 6-di-tert-butyl-4-methylphenol (9.9:0.1, v/v) ether using a blender for 1 min. The extraction solvent was carefully passed through filter paper as it was transferred to a 500 mL separating funnel. And the procedures were repeated for three times. Then the organic layer was collected into a round-bottom flask and evaporated to dryness by a rotary evaporator. The round-bottom flask was washed with acetonitrile:dichloromethane: methanol (7: 2: 1, v/v/v), concentrated to 1 mL and then followed by filtration through 0.45μm membrane filters (millipore). A 20μL aliquot of the resulting solution was then assayed by HPLC. Results The limit of detection and quantitation was 0.088 mg/kg and 0.23 mg/kg, respectively. The developed method exhibited good linearity over the range from 1 to 50 mg/L with a correlation coefficient of 0.9996, and the av-erage recovery was 95.59%. The operation time for sample preparation was about 20 to 25 min. The method was used to detect β-carotene in three apricots and the contents in yellow apricot was proved to be highest. Conclusion The method is convenient, fast, accurate and is suitable for the rapid determination ofβ-carotene in apricots.