摘要
以葡萄柚果实为试材,分别采用三氯乙酸/乙醚、三氯乙酸/三氯甲烷、乙酸乙酯/环己烷提取果皮水杨酸,采用高效液相色谱法测定其含量,筛选得出简单易行的提取及测定葡萄柚果皮水杨酸含量的方法。利用此方法对15 g/L羧甲基壳聚糖(CMC)、200 mg/L水杨酸(SA)单独及复合处理的葡萄柚果皮内源水杨酸含量进行测定分析。结果表明,可采用三氯乙酸/乙醚从葡萄柚果皮提取的水杨酸分离效果较好,测定最佳色谱条件为:Eclipse XDB-C18柱(150 mm×4.6 mm,5μm),流动相0.2 mol/L pH 5.5乙酸钠缓冲溶液—甲醇(40∶60),检测波长296 nm,流速0.8 mL/min,进样量5μL。水杨酸质量浓度在3.91~500μg/mL范围内与峰面积呈现良好的线性关系,处理样品果皮的游离态水杨酸含量范围为18~47.6μg/g,结合态水杨酸含量范围是68.05~73.85μg/g。在室温贮藏的28 d内,相比未处理果实(对照),经诱导处理的游离态水杨酸和结合态水杨酸含量均呈升高的趋势,羧甲基壳聚糖/水杨酸复合处理的游离态水杨酸含量显著高于单独处理含量(P<0.05)。采用三氯乙酸/乙醚提取葡萄柚果皮水杨酸具有较高的分离度,本试验所得HPLC方法简单易行,可以用于葡萄柚果皮内源水杨酸的提取分离和测定。
In the present study,the grapefruit fruits were used as experimental materials,and the salicylic acid was extracted from the peels by trichloroacetic acid/ether,trichloroacetic acid/chloroform and ethyl acetate/cyclohexane,which was determined through high performance liquid chromatography(HPLC),aiming to screen the optimal extraction and determination methods for salicylic acid in grapefruit peels.The method was further applied to determine the endogenous salicylic acid contents after single and compound treatments by carboxymethyl chitosan(CMC)of 15 g/L and salicylic acid(SA)of 200 mg/L.Results showed that,the superior separation effect for salicylic acid was trichloroacetic acid/ether extraction,and the optimal chromatographic conditions were determined as follows:column of Eclipse XDB-C18(150 mm×4.6 mm,5μm),mobile phase of 0.2 mol/L sodium acetate buffer solution-methanol(40∶60)with pH of 5.5,detection wavelength of 296 nm,flow rate of 0.8 mL/min and injection volume of 5μL.SA concentrations showed a good linear relationship in the range of 3.91~500μg/mL,the free and combined salicylic acid contents of grapefruit peels ranged from 18~47.6μg/g and 68.05~273.85μg/g,respectively.During 28 days storage period,compared with the control,the free and bound SA contents in treated fruits showed an increasing trend,and the free SA content after CMC/SA combined treatments was significantly increased compared with that of single treatment.The trichloroacetic acid/ether extraction for salicylic acid from grapefruit peels showed a higher separation degree,and HPLC method obtained in this experiment was simple and feasible,and could be used for the extraction,separation and determination of endogenous salicylic acid from grapefruit peels.
作者
李文清
孔珊珊
马电通
朱绍志
李贤忠
邓佳
LI Wen-qing;KONG Shan-shan;MA Dian-tong;ZHU Shao-zhi;LI Xian-zhong;DENG Jia(Forestry College of Southwest Forestry University,Kunming 650224,China;Key Laboratory of Southwest Forestry University,Ministry of Education,Southwest Mountain Forest Resources Conservation andUtilization,Kunming 650224,China)
出处
《保鲜与加工》
CAS
2021年第6期93-99,106,共8页
Storage and Process
基金
国家自然科学基金资助项目(31960326)
西南山地森林资源保育与利用教育部重点实验室开放课题(KLESWFU—201901)。
关键词
葡萄柚
羧甲基壳聚糖
水杨酸
高效液相色谱法
内源水杨酸
grapefruit
carboxymethyl chitosan
salicylic acid
high performance liquid chromatography
endogenous salicylic acid
