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作 者:邢雅丽[1,2,3,4] 毕良武[1,2,3,4,5] 赵振东[1,2,3,4,5] 韩路路[1,2,3,4] 夏田娟
机构地区:[1]中国林业科学研究院林产化学工业研究所 [2]生物质化学利用国家工程实验室 [3]国家林业局林产化学工程重点开放性实验室 [4]江苏省生物质能源与材料重点实验室,江苏南京210042 [5]中国林业科学研究院林业新技术研究所,北京100091
出 处:《林产化学与工业》2014年第4期37-41,共5页Chemistry and Industry of Forest Products
基 金:国家林业局948技术引进项目(2011-4-01)
摘 要:在考察HPLC流动相体系和色谱柱对熊果酸、齐墩果酸分离测定影响的基础上,采用中心复合设计,以分离度和分析时间为响应值,对熊果酸和齐墩果酸HPLC分离测定的主要影响因素(甲醇与水相的体积比、水相中磷酸的体积分数、流动相流速及柱温)进行多重响应优化,建立了有效、快速的分离测定熊果酸和齐墩果酸的HPLC方法。结果表明,在210 nm的检测波长下,用Shim-pack ODS-CLC(M)色谱柱,流动相为甲醇/磷酸水溶液体系,甲醇与水体积比为91.7∶8.3,磷酸体积分数为0.05%,流速为0.6 mL/min,柱温为21℃,齐墩果酸和熊果酸可以在23 min内得到有效分离,分离度达到1.739。Effects of HPLC mobile phase and column on the separation and determination of ursolic acid and oleanolic acid were in vestigated. By using the resolution and the analysis time as response values, the main influencing factors of HPLC( the volumetric ratio of methanol and aqueous phase in the mobile phase, the volume fraction of phosphoric acid in the aqueous phase, as well as the flow rate of the mobile phase and the column temperature) were optimized by central composite design. An effective and fast method for the separation and determination of ursolic acid and oleanolic acid by HPLC was established. The results showed that oleanolic acid and ursolie acid were effectively separated within 23 min with the resolution of 1. 739, when the chromatographic separation was performed on a Shim-pack ODS-CLC (M) column kept at 21 ℃, using the methanol and aqueous phase containing 0.05 % phosphoric acid with the volumetric ratio of 91. 7 : 8.3 as the mobile phase at a flow rate of 0.6 mL/min, and the detection wavelength was set at 210 nm.
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