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作 者:王文俊[1] 白玮玮[1] 李军超[2] 刘书慧[1,3]
机构地区:[1]西北农林科技大学理学院,陕西杨陵712100 [2]西北农林科技大学生命科学学院,陕西杨陵712100 [3]陕西省农业分子生物学重点实验室,陕西杨陵712100
出 处:《西北植物学报》2011年第9期1894-1899,共6页Acta Botanica Boreali-Occidentalia Sinica
基 金:西北农林科技大学引进人才科研专项项目(01140414)
摘 要:为建立一种加速溶剂萃取-毛细管区带电泳测定女贞子中齐墩果酸和熊果酸的新方法.考察了萃取温度、萃取时间和萃取次数对目标物萃取效率的影响,并考察了硼砂浓度,β-环糊精浓度、pH及甲醇浓度对目标物分离的影响.结果表明:(1)萃取温度和萃取次数影响目标物的萃取效率,而萃取时间的影响很小;萃取压力影响萃取过程的重现性.(2)优化的萃取条件为:萃取压力6.9 MPa,萃取温度100℃,萃取时间5 min和萃取次数2次.(3)优化的缓冲体系为:40 mmol/L硼砂,1 mmol/Lβ-环糊精,pH 9.5及6%甲醇.(4)齐墩果酸和熊果酸分别在10-200、10-160 mg/L范围内线性良好,相关系数均大于0.996,检测限分别为3.2 mg/L和3.0 mg/L,加标回收率为93%-97%.对比了加速溶剂萃取、索氏提取以及超声提取的提取效率.(5)不同提取方法比较结果表明,加速溶剂萃取的提取效率与索氏提取法接近,但高于超声提取;加速溶剂萃取法的主要优点是消耗提取溶剂量少,提取时间短,样品用量小.A new method for the determination of oleanolic acid(OA) and ursolic acid(UA) in Ligustrum lucidum Ait using accelerated solvent extraction(ASE) combined with capillary zone electrophoresis(CZE) has been developed.The effects of important operational parameters,such as extraction temperature,time,pressure and cycle,on the performance of ASE were investigated and optimized.Extraction temperature and cycle times influenced the extraction efficiency considerably,and no obvious effect of extraction time on efficiency was observed.Interestingly,the results showed extraction pressure played an important role in the reproducibility of the extraction process.The optimum extraction conditions included an extraction pressure of 6.9 MPa,an extraction temperature of 100℃ and a static extraction time of 5 min with 2 cycles.The parameters influencing the separation efficiency of capillary electrophoresis were observed,and the optimum buffer system was 40 mmol/L borax,1 mmol/L beta cyclodextrin,pH 9.5 and 6% methanol.The good linearity was obtained for oleanolic acid and ursolic acid in the range of 10-200 mg/L and 10-160 mg/L,respectively,with the correlation coefficient over 0.996.The limits of detection ranged from 3.2 mg/L to 3.0 mg/L,and the recoveries from 93 to 97%.The contents of OA and UA in L.lucidum extracted by ASE were compared with that from Soxhlet and sonication extraction.
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