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

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×250 mm,5μm)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0.6 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,R^(2)>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。

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-504E(4.6 mm×250 mm,5μm)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 10μL.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 R^(2)>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.