基于HPLC-CAD的元胡止痛口服液糖类成分定量指纹图谱研究
Development of a Quantitative Chromatographic Fingerprint Analysis Method for Sugar Components of Yuanhu Zhitong Oral Liquid Using HPLC-CAD
兰婧 1颉佳乐 1曹智铭 2关建丽 2王毅 3龚行楚3
作者信息
- 1. 浙江大学药学院,杭州 310058;浙江大学智能创新药物研究院,杭州 310018
- 2. 河南福森药业有限公司,南阳 474450
- 3. 浙江大学药学院,杭州 310058;浙江大学智能创新药物研究院,杭州 310018;现代中药创制全国重点实验室,杭州 310058
- 折叠
摘要
目的 采用高效液相色谱-电喷雾检测器(HPLC-CAD)检测技术建立元胡止痛口服液中糖类成分的定量指纹图谱分析方法.方法 采用NH2P-504E(4.6 mm×250mm,5 μm)色谱柱,以水(A)-乙腈(B)为流动相进行梯度洗脱,柱温为30℃,进样量为10μL,流速为0.6mL·min-1,CAD雾化温度为35℃,采样频率10Hz,幂函数1.0.结果 定量成分在定量范围内线性关系良好,R2＞0.999,仪器精密度、中间精密度、方法重复性的RSD均＜3％,供试品溶液在24 h内稳定,低、中、高3个浓度水平的平均加样回收率为97.15％～101.13％.指纹图谱中含共有峰5个,其仪器精密度、重复性、稳定性的RSD值均＜4％.结论 建立的分析方法稳定、准确、重复性好,能够检测制剂中的糖类辅料.
Abstract
OBJECTIVE To establish a quantitative fingerprint analysis method for sugar components in Yuanhu Zhitong oral liquid using high performance liquid chromatography-charged aerosol detection(HPLC-CAD).METHODS Chromatographic column was NH2P-50 4E(4.6 mm×250 mm,5 μm)column.Water(A)and acetonitrile(B)were used as the mobile phase in the gradient elute mode.The column temperature was 30 ℃.The injection volume was 10 μL.The flow rate was 0.6 mL·min-1.The evaporation temperature of CAD was 35 ℃.The acquisition frequency was 10 Hz.The power function value was l.0.RESULTS The linear relationship of the quantitative component was good within the quantitative range,with R2＞0.999.The relative standard deviations(RSDs)of instrument precision,intermediate precision and method repeatability were all＜3％.The test solution was stable within 24 h.The average recoveries at low,medium and high concentration levels ranged 97.15％-101.13％.There were 5 common peaks in the fingerprint.The RSDs of instrument precision,method repeatability and sample stability were all＜4％.CONCLUSION The established analytical method is stable,accurate and reproducible.It can be used to detect sugar excipients in the preparations.
关键词
高效液相色谱-电喷雾检测器/元胡止痛口服液/糖类/定量指纹图谱Key words
HPLC-CAD/Yuanhu Zhitong oral liquid/sugar/quantitative chromatographic fingerprint引用本文复制引用
基金项目
国家中医药管理局创新团队与人才支持计划(ZYYCXTD-D-202002)
河南省重大科技专项项目(201111310800)
出版年
2024
NETL
NSTL
万方数据