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作 者:牛林林 李溢真 陈勉 袁丹丹 尉茜 孔令斌 王传金 刘英梅 刘峰 刘飞 张岱州 NIU Lin-lin;LI Yi-zhen;CHEN Mian;YUAN Dan-dan;WEI Qian;KONG Ling-bin;WANG Chuan-jin;LIU Ying-Mei;LIU Feng;LIU Fei;ZHANG Dai-zhou(Shandong Academy of Pharmaceutical Sciences,Shandong Engineering Research Center for Efficient Preparation and Application of Sugar and Sugar Complex,Shandong Key Laboratory of Human Vaccine Research and Development(Preparatory),National Local Joint Engineering Laboratory for Polysaccharide Drug Fermentation and Refinement,Jinan 250101,China;Shandong Academy of Biomedical Sciences Co.,Ltd.,Jinan 250101,China)
机构地区:[1]山东省药学科学院,糖及糖复合物高效制备及应用山东省工程研究中心,山东省人用疫苗研发重点实验室(筹),多糖类药物发酵与精制国家地方联合工程实验室,山东济南250101 [2]山东省生物医药科学院有限公司,山东济南250101
出 处:《食品与药品》2025年第1期52-56,共5页Food and Drug
基 金:山东省重点研发计划(编号:2021SFGC1205),山东省重大科技创新(编号:2021ZDSYS07),山东省科技型中小企业创新能力提升工程项目(编号:2022TSGC1006),济南市高校院所创新团队项目(编号:202228040)。
摘 要:目的建立高效液相色谱法测定去皮罗汉参和罗汉参皮中西瑞香素含量的方法。方法以西瑞香素含量为评价指标,采用正交试验考察了乙醇用量、超声次数、超声时间、超声温度对罗汉参中西瑞香素的影响,筛选最佳提取工艺。采用XDB-C_(18)色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.2%磷酸水溶液(55:45)为流动相,等度洗脱,检测波长为346 nm,流速为1.0 ml/min,柱温为35℃。结果西瑞香素浓度在5~100μg/ml范围内与色谱峰面积呈良好的线性关系,回归方程为Y=66750X-68446,r=0.9984。定量限(S/N=10)为0.025μg/ml,检测限(S/N=3)为5 ng/ml。方法的重复性(n=6)、中间精密度(n=12)、稳定性(n=6)RSD均≤2%,去皮罗汉参和罗汉参皮的平均加标回收率分别为106.23%,97.26%,RSD分别为0.62%,1.5%。结论该方法重复性好、准确度高,可作为罗汉参质量控制方法。Objective To establish an HPLC method for the determination of daphnoretin in Luohanshen peel and peeled Luohanshen.Methods With the content of daphnoretin as the evaluation index,the effects of ethanol dosage,and ultrasonic treatment times,time and temperature on daphnoretin in Luohanshen were investigated by orthogonal experiment,and the best extraction process was screened out.The determination was performed on an XDB-C_(18) column(4.6 mm×250 mm,5μm),using methanol-0.2%phosphoric acid aqueous solution(55:45)as mobile phase of isocratic elution.The detection wavelength was 346 nm,the flow rate was 1.0 ml/min,and the column temperature was 35℃.Results The concentration of daphnoretin in the range of 5-100μg/ml showed a good linear relationship with the chromatographic peak area,and the regression equation was:Y=66750X-68446(r=0.9984).The limit of quantification(S/N=10)was 0.025μg/ml,and the limit of detection(S/N=3)was 5 ng/ml.The RSDs of s of repeatability test(n=6),intermediate precision test(n=12)and stability test(n=6)were all less than 2%.The average recoveries of daphnoretin in Luohanshen peel and peeled Luohanshen were 106.23%,97.26%,and the RSDs were 0.62%and 1.5%,respectively.Conclusion The method has good repeatability,high accuracy,and can be used as a quality control method for Luohanshen.
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