摘要
目的建立测定参麦降糖片中马钱苷含量的方法。方法采用高效液相色谱法,设置参数色谱柱为Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm)、流动相为乙腈-水(10∶90)、柱温25℃、检测波长240 nm、流速1.0 mL/min。取对照品溶液、供试品溶液、阴性对照溶液,按设定的色谱条件,分别进样10μL,进行一系列试验,实时记录色谱图。结果 (1)根据系统适用性试验的色谱图,对照品溶液和供试品溶液在保留时间22.9 min处出色谱峰,而阴性对照溶液中并未可见色谱峰,说明马钱苷的测定不受其他杂质峰的干扰,专属性好;(2)线性关系:马钱苷进样量在0.10~0.52μg范围内线性关系良好(r=0.999 5);(3)精密度:马钱苷峰面积值的RSD值为0.22%(n=6),表明本法精密度良好;(4)稳定性:马钱苷峰面积值的RSD值为1.20%(n=5),表明在8 h内供试品溶液保持稳定;(5)重复性:马钱苷含量的RSD=0.83%,表明重现性较好;(6)加样回收率:平均回收率99.87%(RSD=0.55%);(7)样品中马钱苷含量:6批样品的平均含量0.936 mg/g,RSD%0.02%,考虑到不同批次的制剂含量因原料和工艺不稳定而存在浮动,故取含量均值的90%作为含量标准的下限,规定本品每片含山茱萸以马钱苷(C17H26O10)计,不得少于0.27 mg,作为本制剂HPLC法含量测定马钱苷的内控标准。结论所建立的方法操作简便、准确可靠,能有效控制参麦降糖片中马钱苷的质量。
Objective To establish a method for the determination of loganin in Shenmai Jiangtang Tablets. Methods High performance liquid chromatography (HPLC) was used. The parameter column was Agilent Zorbax sb-C18 (250 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile water (10∶90). The column temperature was 25 ℃. The detection wavelength was 240 nm and the flow rate was 1. 0 mL/min. The control solution,test solution and negative control solution were respectively injected 10 μL according to the set chromatographic conditions. We carried out a series of tests,and recorded the chromatogram in real time. Results (1) According to the chromatogram of the system suitability test,the excellent peaks were found in the reference solution and the test solution at the retention time of 22. 9 min,but no peaks were found in the negative control solution,indicating that the determination of loganin was not interfered by other impurity peaks and had good specificity. (2) Linear relationship: The linear relationship was good within the range of 0. 10 ~ 0. 52 μg (r = 0. 999 5). (3) Precision: The RSD value of loganin peak area value was 0. 22% (n = 6),indicating that the precision of this method was good. (4) Stability: The RSD value of loganin peak area value was 1. 20% (n = 5),indicating that the test solution remained stable within 8 hours. (5) Repeatability: The RSD value of loganin content was 0. 83%,indicating good reproducibility. (6) Sample addition recovery: The average recovery rate was 99. 87% (RSD = 0. 55%). (7) The content of loganin in the sample: The average content of 6 batches of samples was 0. 936 mg/g and RSD valuewas 0. 02%,considering that the content of different batches of preparations fluctuates was due to the instability of raw materials and processed products,90% of the average content was taken as the lower limit of the content standard. It is stipulated that each tablet containing Cornus officinaliscalculated by loganin (C17H26O10) not less than 0. 27 mg,which is used as the HPLC content determi
作者
王汝山
林锐
WANG Rushan;LIN Rui(Yangjiang Hospital of Traditional Chinese Medicine,Yangjiang 529500,Guangdong,China;Yangjiang Testing Center,Yangjiang 529500,Guangdong,China)
出处
《实用中医内科杂志》
2020年第12期109-111,共3页
Journal of Practical Traditional Chinese Internal Medicine
关键词
高效液相色谱法
参麦降糖片
山茱萸
马钱苷
含量测定
实验研究
内控标准
质量控制
HPLC
Shenmai Jiangtang Tablet
Cornus officinalis
loganin
content determination
experimental study
internal control standard
quality control
