复方桔梗止咳片的质量标准研究

Study on Quality Standard of Compound Platycodon grandiflorum Antitussive Tablets

目的:建立复方桔梗止咳片的质量标准。方法:采用薄层色谱法(TLC)对复方桔梗止咳片中桔梗、远志、甘草进行定性鉴别;采用高效液相色谱法-蒸发光散射检测法测定复方桔梗止咳片中桔梗皂苷D的含量。色谱柱为Agilent C18,流动相为乙腈-水(26∶74,V/V),流速为1.0 mL/min,检测器为蒸发光散射检测器,漂移管温度为105℃,载气流速为3.0 L/min,柱温为35℃。结果:桔梗、远志、甘草的TLC图谱中斑点清晰,分离度好,阴性对照未见相同斑点。桔梗皂苷D的进样量线性范围为0.4219~5.0628μg(r=0.9999);定量限、检测限分别为0.364、0.109μg;精密度、稳定性、重复性、耐用性试验的RSD均小于3.0%;加样回收率为87.32%~91.96%(RSD=1.73%,n=6)。178批样品中,桔梗皂苷D的含量为0.004~0.73 mg/片,有55批(30.9%)样品中桔梗皂苷D含量低于本研究拟定的含量限度(0.10 mg/片)。结论:所建质量标准方法准确、可靠,可用于复方桔梗止咳片的质量控制。

OBJECTIVE:To establish the quality standard of Compound Platycodon grandiflorum antitussive tablets.METHODS:TLC was used to identify the P.grandiflorum,Polygala tenuifolia and Glycyrrhiza uralensis qualitatively in Compound P.grandiflorum antitussive tablets.HPLC-ELSD method was used to measure the content of platycodin D in Compound P.grandiflorum antitussive tablets.The determination was performed on Agilent C18 column with mobile phase consisted of acetonitrile-water(26∶74,V/V)at the flow rate of 1.0 mL/min.ELSD was used with drift tube temperature of 105℃,gas flow rate of 3.0 L/min and column temperature at 35℃.RESULTS:TLC chromatograms of P.grandiflorum,P.tenuifolia and G.uralensis had clear spots with good separation and no same spot from negative samples.The linear range of platycodin D was 0.4219-5.0628μg(r=0.9999).The quantitative limit and detection limit were 0.364,0.109μg,respectively.RSDs of precision,stability,reproducibility and durability tests were all lower than 3.0%.The recovery rates were 87.32%-91.96%(RSD=1.73%,n=6).The platycodin D contents of 178 samples ranged from 0.004 to 0.73 mg/tablet.The content of platycodin D in 55 batches(30.9%)of samples was lower than the content limit(0.10 mg/tablet)proposed in this study.CONCLUSIONS:Established method is accurate and reliable,and can be used for the quality control of Compound P.grandiflorum antitussive tablets.