摘要:
目的 采用高效液相色谱-蒸发光散射法(HPLC-ELSD)测定膜荚黄芪中黄芪甲苷的含量方法 黄芪药材经甲醇-氨水(v/v 9:1)超声提取,确定实验条件并进行方法学考察,色谱条件:依利特Hypersil ODS 2 色谱柱(4.6mm×250mm,5μm);流动相:A相为乙腈,B相为水,梯度洗脱;流速:1.0mL/min;柱温;室温;进样量:20μL.ELSD检测器条件:漂移管温度:40℃,载气(空气)压力:3.5Bar,增益值:7 结果 方法学考察结果表明,黄芪甲苷低、中、高3个进样量的日内精密度和日间精密度的RSD均小于2.0%,48h内稳定性试验的RSD分别为1.24%,重复性试验的RSD分别为1.26%(n=5),最低检测限分别为0.6930mg/mL,加样回收率结果分别为97.05%,RSD=0.17%(n=3) 膜荚黄芪中黄芪甲苷的含量均符合药典标准讨论:该方法缩减了黄芪药材的前处理步骤,测定结果准确,能够用于黄芪药材中黄芪甲苷含量测定的研究
Abstract:
Objective To determine astragaloside Ⅳ in Radix Astragali by HPLC-KLSD. Methods Radix Astragali was extracted with MeOH-NH3·H2O(v/v 9:1),the condition was confirmed and the validation of the method was also tested. The chromatogra phy condition was with Hypersil ODS 2 column (4.6mm×250mm,5μm); mobile phase was A; ACN,B:H2O, gradient elutron,flow speed was 1.0 ml/min, temperature of column was room temperature, inject volume:20μL. The KLSD conditions were as follows:the temperature of drift tube was 40℃, the gas pressure was 3.5Bar, the value of gain was 7. Results The intra-day and mter-day precision (RSD)at low, middle and high injection amount were all less than 2.0%. The stability (RSD) was 1.24% in 48h. The recuerence (RSD, n=5) was 1.26%. The limit of detection was 0.6930mg/mL The recoveries were 97.05% (KSD=0.17%, n=3) for astragaloside Ⅳ. The contents of astragaloside Ⅳ in (en different batch of Astragalus membranaceus (Fisch.) Bge. were accord to the standard of Chinese Pharmacopoeia. Conclusion The method covild shorten the process and time of Radix Astragali pretreatment with character of simple, suitable and reliable. The studies could apply to determine the content of astragaloside Ⅳ in Radix Astragalt.
点击查看大图
下载:
