高效液相色谱法测定冬凌利咽糖浆中冬凌草甲素含量  

Content Determination of Oridonin in Dongling Liyan Syrup by HPLC Method

作　　者：陈玉璞 CHEN Yupu(Jiaozuo Food and Drug Inspection Institute,Jiaozuo 454000,Henan,China)

机构地区：[1]焦作市食品药品检验所,河南焦作454000

出　　处：《实用中医内科杂志》2020年第2期105-108,共4页Journal of Practical Traditional Chinese Internal Medicine

摘　　要：目的建立测定冬凌利咽糖浆中冬凌草甲素含量的方法。方法运用高效液相色谱法,设置参数色谱柱为250 mm×4.6 mm,5μm的C18柱、55∶45比例甲醇-水流动相、1.00 mL/min流速、239 nm检测波长。分别完成对照品、待试品、阴性对照3种不同液体精密吸取,并设定以上色谱条件,取出10μL液相色谱仪器置入其中,实时记录色谱图结果。结果(1)根据记录的色谱图能够发现,处于此种色谱条件下能够在时间达到4.1 min处保留时间,对比待试品以及对照品两种溶液产生色谱峰,但是在阴性对照溶液中,并未可见色谱峰。说明冬凌草甲素的测定不受其它杂质峰的干扰。(2)冬凌草甲素在0.60~12.00 mg/L浓度范围内线性关系良好(r=0.9999);(3)平均回收率98.1%,RSD=1.53%;(4)稳定性:冬凌草甲素峰面积的相对标准偏差(relative standard deviation,RSD)=0.79%,表明供试品溶液在24 h内稳定性良好;(5)重复性:冬凌草甲素含量的RSD=0.83%,表明重现性较好。(6)冬凌草甲素含量:批号20180105冬凌草甲素含量为0.43 g/L,RSD为0.96%,批号20180323冬凌草甲素含量为0.38 g/L,RSD为1.12%,批号20180511冬凌草甲素含量为0.40 g/L,RSD为1.03%。结论目前,高效液相色谱法仍然是分析冬凌草中冬凌草甲素最常应用的方法之一,但随着技术的发展,UPLC方法的应用也会越来越普及。方法简便、快速、准确,专属性强,能够对于测量冬凌利咽糖浆中的冬凌草甲素含量准确检测,确保检测结果相符实际的药物含量,因此可用于冬凌利咽糖浆中冬凌草甲素含量测定。Objective To establish a method for the determination of oridonin in Dongling Liyan Syrup.Methods HPLC was used to set the parameter column as 250 mm×4.6 mm,5μm C18 column,55:45 ratio methanol-water mobile phase,1.00 mL/min flow rate,and 239 nm detection wavelength.The precise absorption of three different liquids(reference solution,to be tested solution and negative control solution)was completed,and the above chromatographic conditions were set.10μL liquid chromatography instrument was taken out and put into the instrument and the chromatographic results were recorded in real time.Results(1)According to the recorded chromatogram,it can be found that under such chromatographic conditions,the retention time can reach 4.1 min,and the chromatographic peak can be generated by comparing the to be tested solution and the control solution,but no chromatographic peak can be seen in the negative control solution.The results showed that the determination of oridonin was not disturbed by other impurity peaks.(2)The oridonin had a good linear relationship within the concentration range of 0.60~12.00mg/L(r=0.9999).(3)The average recovery rate was 98.1%with RSD=1.53%.(4)Stability:The relative standard deviation(RSD)of the peak area of rabdosia rubescens=0.79%,indicating that the tested solution had a good stability within 24 h.(5)Repeatability:The RSD of oridonin content was 0.83%,indicating good reproducibility.(6)Oridonin content:The oridonin content of batch 20180105 was 0.43 g/L with RSD=0.96%.The oridonin content of batch 20180323 was 0.38 g/L with RSD=1.12%.The oridonin content of batch 20180511 was 0.40 g/L with RSD=1.03%.Conclusion At present,HPLC is still one of the most commonly-used methods for the analysis of rubeshaidin in rabdosia rubeshaidae,but with the development of technology,the application of UPLC method will be more and more popular.This method is simple,rapid,accurate and specific.It can accurately detect the content of oridonin in the syrup and ensure that the detection results are consistent with t

关 键 词：高效液相色谱法 冬凌利咽糖浆 冬凌草甲素 含量 

分 类 号：R927.2[医药卫生—药学]