Determination of Oleanolic Acid in Quinoa by High Performance Liquid Chromatography
摘 要
建立了高效液相色谱法(HPLC)测定藜麦中齐墩果酸含量的方法。称取藜麦样品1.5 g,用甲醇40 mL和3 mol·L-1盐酸溶液10 mL溶解,超声提取20 min,再回流水解1.5 h,将其中的齐墩果酸转化成苷元,以排除杂质干扰。所得提取液以体积比为85:15的甲醇-0.1 mol·L-1乙酸铵溶液的混合液为流动相,采用HPLC分离并测定样品提取液中齐墩果酸的含量。结果表明:齐墩果酸的质量浓度在5~500 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.3 mg·kg-1;对藜麦样品进行3个浓度水平的加标回收试验,齐墩果酸的回收率为98.0%~101%,测定值的相对标准偏差(RSD,n=5)为4.2%~7.5%。方法用于12个实际样品的测定,齐墩果酸的检出量为0.51~21.26 g·kg-1。
Abstract
A method for determination of oleanolic acid in quinoa by high performance liquid chromatography (HPLC) was established. Quinoa sample of 1.5 g was dissolved in 40 mL of methanol and 10 mL of 3 mol·L-1 hydrochloric acid solution, and oleanolic acid was extracted by ultrasonic for 20 min, following by reflux hydrolysis for 1.5 h, which could convert oleanolic acid into aglycone in order to avoid the interference of impurities. A mixture of methanol and 0.1 mol·L-1 ammonium acetate solution at volume ratio of 85:15 was used as the mobile phase, and the content of oleanolic acid in the sample extract was determined by HPLC. As shown by the results, linear relationship between mass concentration of oleanolic acid and its peak area was kept in the range of 5-500 mg·L-1, with detection limit (3S/N) of 0.3 mg·kg-1. Recovery test was made on quinoa samples at 3 concentration levels by standard addition method, giving results in the range of 98.0%-101%, and RSDs (n=5) of the determined values ranged from 4.2% to 7.5%. This method was applied for determination of oleanolic acid in 12 actual samples, and the detection amounts of oleanolic acid were in the range of 0.51-21.26 g·kg-1.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202112011
所属栏目 工作简报
基金项目 宁夏自然科学基金项目(NZ17264);宁夏农林科学院科技创新引导项目(NKYG-17-06)
收稿日期 2020/7/8
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联系人作者王芳(572865067@qq.com)
备注田建文,博士,主要从事农产品质量的相关研究工作
引用该论文: TIAN Jianwen,WANG Caiyan,WANG Fang,ZHAO Zidan. Determination of Oleanolic Acid in Quinoa by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(12): 1119~1122
田建文,王彩艳,王芳,赵子丹. 高效液相色谱法测定藜麦中齐墩果酸的含量[J]. 理化检验-化学分册, 2021, 57(12): 1119~1122
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【2】马维亮.宁夏藜麦规模化发展现状及建议[J].宁夏农林科技, 2017,58(8):48-49.
【3】王黎明,马宁,李颂,等.藜麦的营养价值及其应用前景[J].食品工业科技, 2014,35(1):381-384.
【4】焦红艳,高文庚,陈丽文.藜麦营养成分测定及对孕期妇女健康的促进作用[J].基层医学论坛, 2018,22(14):1902-1903.
【5】任卓伟,倪文杰,刘森.藜麦皂甙的测定研究[J].山西农业科学, 2015,43(8):932-935.
【6】KULJANABHAGAVAD T, WINK M. Biological activities and chemistry of saponins from Chenopodium quinoa Willd.[J]. Phytochemistry Reviews, 2009,8(2):473-490.
【7】赵文婷.藜麦麸皮总皂苷的提取纯化及其抗氧化和免疫增强作用[D].晋中:山西农业大学, 2015.
【8】董玉秀,邓向涛.连钱草中熊果酸与齐墩果酸测定方法研究[C]//中国药学会中药与天然药物专业委员会.第十届全国中药和天然药物学术研讨会论文集.洛阳:[出版者不详], 2009:334-337.
【9】周志勇,袁丁.齐墩果酸药理作用研究进展[J].中国医院药学杂志, 2008,28(23):2031-2033.
【10】李必波,赵领,张雪梅,等.紫外光谱法测定齐墩果酸缓释滴丸药物含量及体外释放度[J].重庆医科大学学报, 2009,34(4):447-451.
【11】牛之瑞,王秀君,于毅涛,等.液相色谱-质谱联用同时测定白酒中8种甜味剂[J].食品科学, 2016,37(2):178-181.
【12】PERES R G, MORAES E P, MICKE G A, et al. Rapid method for the determination of organic acids in wine by capillary electrophoresis with indirect UV detection[J]. Food Control, 2009,20(6):548-552.
【13】付亚玲,高琳,张东旭,等.齐墩果酸和熊果酸提取、分离与测定方法研究进展[J].食品研究与开发, 2020,41(2):196-199.
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