水果果实中主要有机酸提取条件的优化

doi:10.3864/j.issn.0578-1752.2014.13.014

摘要/Abstract

摘要： 【目的】建立一种能同时测定水果果实中主要有机酸（柠檬酸、酒石酸、苹果酸、琥珀酸）含量的有效提取方法。【方法】以柑橘、葡萄等为试材，以乙醇的水溶液为提取剂，采用超声提取的方法，对提取剂提取效果（乙醇溶液浓度配比、纯水提取效果及主要有机酸的稳定性、不同浓度乙醇溶液提取效果、10%乙醇溶液提取效果及主要有机酸的稳定性等）、提取条件（提取方式、超声提取时间等）进行优化试验研究。用优化的提取方法对方法技术参数（检出限、精密度、重复性、准确度等）进行测试，并将测定结果与已有国标法测定结果进行比较分析。【结果】水果果实中有机酸提取的适宜方法为乙醇溶液超声提取法：样品用10%乙醇溶液在超声波提取器中提取30 min，提取后加入硫酸溶液，使提取液中含有和流动相一致的硫酸质量浓度，然后用10%乙醇溶液定容，混匀后离心过滤。取部分滤液用0.22 μm水性滤膜针头过滤器过滤，供离子色谱分析用。在此条件下，主要有机酸提取完全，且提取液在室温条件下稳定性好，至少在15 d内各主要有机酸不会转变为乳酸和乙酸。优化后的提取方法精密度高（RSD为0.28%—1.20%），重复性好（变异系数为0.236%—3.02%（n=5）），准确度高（回收率为88.9%—101.2%），有机酸组分测定效果优于已有国标测定结果。【结论】该方法快速、简便，准确度高、重现性好，适合水果果实中主要有机酸含量的测定。

关键词: 水果 , 有机酸 , 乙醇 , 提取 , 离子色谱

Abstract: 【Objective】This study aimed at investigating an effective extraction method of main organic acids(citric acid, tartaric acid, malic acid, succinic acid) from fruits.【Method】Using citrus, grapes and other fruits as test materials, the aqueous ethanol solution as the extraction agent, and using ultrasonic extraction method, the effect of extraction on the extraction agent (ethanol concentration, ratio of water extraction and organic acid stability, different concentrations of ethanol extraction, effect of 10% ethanol soluble extractant and the main organic acid stability and so on), extraction conditions (extraction method, ultrasonic extraction time and so on) were studied for optimization. Technical parameters for optimized extraction conditions (the detection limit, precision, repeatability, accuracy) were tested. The measuring results by using this method were compared with analytical results with the existing national standard method.【Result】The suitable method for organic acid extraction in fruits is the ethanol ultrasonic extraction method: Samples were extracted for 30 min with 10% ethanol solution in ultrasonic extractor. Then sulfuric acid solution was added, the concentration of sulfuric acid contained in solution was the same as in flow consistent solution. Finally constant volume was made with ethanol solution, then mixed and filtered. The filtrate was filtered by 0.22 μm aqueous membrane needle filter for ion chromatography analysis. All the main organic acids could be extracted completely. The main organic acids didn’t change to lactic acid and acetic acid at least in 15 days when the extract was placed under natural conditions. The optimized extraction method is high precision (RSD 0.28%-1.20%), repeatability (variation coefficient of 0.236%-3.02% (n=5)) and high accuracy (recovery 88.9%-101.2%). The method of organic acids in the determination results was significantly higher than the existing national standard results.【Conclusion】The method was rapid, simple, accurate, reproducible, and suitable for the determination of the contents of main organic acid in fruits.

Key words: fruit , organic acid , ethanol , extract , ion chromatography

庞荣丽, 方金豹, 郭琳琳, 谢汉忠. 水果果实中主要有机酸提取条件的优化[J]. 中国农业科学, 2014, 47(13): 2625-2633.

PANG Rong-Li, FANG Jin-Bao, GUO Lin-Lin, XIE Han-Zhong. Extraction Conditions Optimization of Main Organic Acids from Fruits[J]. Scientia Agricultura Sinica, 2014, 47(13): 2625-2633.

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