摘要
目的建立中药钩藤中钩藤碱的高效液相色谱-蒸发散射检测器法(HPLC-ELSD)的测定方法。方法采用甲醇冷浸超声法处理钩藤药材,经0.22μm的滤膜过滤后进样分析;色谱柱为Diamonsil C18(4.6mm×200mm,5μm),流动相组成,乙腈:0.01mol/L醋酸铵=20∶80,采用梯度洗脱方式,乙腈比例在20min内从20%变为60%,流速为1.0mL/min,柱温为室温30℃,进样量为20μL。ELSD参数:飘移管温度105℃,载气(N2)流速3.0mL/min。结果钩藤碱测定的浓度范围内呈良好线性(r=0.999 0),加标回收率大于96.1%,日内、日间变异系数均小于8.0%,重复性试验RSD为4.7%,稳定性试验钩藤碱高、中、低浓度溶液室温48h内RSD为6.8%、7.2%、9.1%。结论该方法成功地应用于钩藤碱含量的测定,成为一个全面评价钩藤质量的新方法。
Objective To establish a method using HPLC-ELSD to determine rhynchophylline in a traditional Chinese herb,Uncaria rhynchophylla.Methods Cold maceration with methanol and supersonic extraction was used to treat the medical material,and the supernatant was filtered through a 0.22 μm membrane.Chromatography was performed on a diamonsil C18（4.6 mm×200 mm,5 μm）.The mobile phase was consisted of acetonitrile（0.01 mol/L） and ammonium acetate[20∶80（V∶V）];then the proportion of acetonitrile changed from 20 % to 60% within 20min by using gradient elution method,the flow rate was 1.0mL/min,the column temperature was 30 ℃ and the sample size was 20 μL.ELSD： the tube temperature was 105 ℃,the nitrogen flow rate was 3.0 mL/min.Results The calibration curve was linear（r=0.999 0） among the concentration range,the recovery of the method was higher than 96.1%,the coefficients of variation for inter day and intra day were both lower than 8.0%,the relative standard deviation（RSD） of the reproducibility test was 4.7% and the stability test was 6.8%、7.2% and 9.1% from the high density to the low.Conclusion As an accurate and reliable method,it can be used for determining rhynchophylline in uncariar rhynchophylla.
出处
《重庆医学》
CAS
CSCD
北大核心
2013年第10期1089-1091,1094,共4页
Chongqing medicine
