基于HPLC-CAD的元胡止痛口服液糖类成分定量指纹图谱研究

兰婧; 颉佳乐; 曹智铭; 关建丽; 王毅; 龚行楚

doi:10.13748/j.cnki.issn1007-7693.20230275

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

摘要

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-50 4E(4.6 mm×250 mm，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10 μL，流速为0.6 mL·min⁻¹，CAD雾化温度为35 ℃，采样频率10 Hz，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 1.0.
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.

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