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食品研究与开发:2017,38(14):155-160
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甜茶中齐墩果酸及熊果酸的检测方法的建立
谭冬明1,石相莉1,*,罗星晔2,农彦贤1,梁炜1,黄健1
(1.桂林市产品质量检验所,广西 桂林 541004;2.桂林市环境监测中心站,广西 桂林 541002)
Establishment for the Determination of Oleanolic Acid and Ursolic Acid from Rubus Suavissimus S.Lee
TAN Dong-ming1, SHI Xiang-li1,*, LUO Xing-ye2, NONG Yan-xian1, LIANG Wei1, HUANG Jian1
(1. Guilin Product Quality Testing Institute, Guilin 541004, Guangxi, China; 2. Guilin Environmental Monitoring Center, Guilin 541002, Guangxi, China)
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投稿时间:2017-04-05    
中文摘要: 建立测定甜茶中齐墩果酸及熊果酸的高效液相色谱分析方法。 对色谱分析条件及样品前处理进行优化研 究,样品经乙醇超声波提取,醇提水沉进行杂质沉淀,以 Hypersil Gold C18(250 mm×4.6 mm,5 μm)为分析柱,甲醇和0.2 %乙酸铵溶液(83 ∶ 17)为流动相,检测波长为 210 nm,流速为 0.6 mL/min,外标法进行定量。在此条件下,齐墩果酸 及熊果酸能达到完全基线分离, 分别在 2.23 μg/mL~112 μg/mL、1.84 μg/mL~92 μg/mL 浓度范围内具有良好的线性关 系(R2>0.999),方法检出限分别为 0.04、0.08 g/kg。在低中高 3 种含量添加水平的回收率在 92 %~102 %,RSD(n=6)为0.8 %~3.8 %。
中文关键词: 甜茶  齐墩果酸  熊果酸  高效液相色谱
Abstract:A method was proposed for the determination of oleanolic acid and ursolic acid from Rubus suavis- simus S.Lee by high performance liquid chromatography. The optimization of chromatographic analysis condition and sample pretreatment were studied. The sample was extracted by ethanol. The impurity was removed by ethanol extraction and water precipitation. The separation was completed by using Hypersil Gold C18(250 mm× 4.6 mm,5 μm)column with carbinol and 0.2 % acetic ammonium solution (83 ∶ 17) as the mobile phase at a flow rate of 0.6 mL/min, and the detection wavelength was 210 nm. The quantification was performed by the ex- ternal standard method. Under these conditions, oleanolic acid and ursolic acid were completely separated, and it showed good linearities with their concentrations ranged from 2.23 μg/mL to 112 μg/mL and from 1.84 μg/mL to 92 μg/mL with correlation coefficients(R2)more than 0.999, and the detection limits were 0.04 and 0.08 g/kg. The recoveries were in the range of 92 %-102 % at 3 spiked levels with RSDs(n=6)of 0.8 %-3.8 %.
文章编号:201714033     中图分类号:    文献标志码:A
基金项目:桂林市科技攻关项目(2016010307)
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