安肠液质量标准的建立

Quality Standard of Anchang Liquid

目的建立安肠液的质量标准。方法采用薄层色谱(TLC)法对制剂中木香、黄芪、白术、甘草进行定性鉴别,并对乌头双酯型生物碱进行限量检查;采用高效液相色谱-蒸发光散射检测法测定制剂中黄芪甲苷含量,色谱柱为Shimadzu Shim-packCLC-ODS柱(150 mm×6.0 mm,5μm),流动相为乙腈-水(38∶62,V/V),流速为1.0 mL/min,检测波长为365 nm,柱温为32℃,进样量为20μL,氮气流速为2.8 L/min,漂移管温度为55℃,增益为2。结果木香、黄芪、白术、甘草的TLC图斑点清晰,分离度好,阴性对照无干扰。乌头双酯型生物碱检测限为7.5μg。黄芪甲苷质量浓度在0.0241~0.3856 mg/mL范围内与峰面积线性关系良好(r=0.9996,n=5);精密度、稳定性、重复性试验结果的RSD均小于2.3%;平均加样回收率为97.35%,RSD为2.03%(n=9)。结论所建立的质量标准准确、可靠,可于安肠液的质量控制。

Objective To establish the quality standard of Anchang Liquid.Methods Thin layer chromatography(TLC)method was used for the qualitative identification of Aucklandiae Radix,Astragali Radix,Atractylodis Macrocephalae Rhizoma,Glycyrrhizae Radix et Rhizoma and the limits of aconite diester-alkaloids in the preparation.High-performance liquid chromatography-evaporative light scattering detection(HPLC-ELSD)method was used for the content determination of astragalosideⅣin Anchang Liquid,the chromatographic column was Shimadzu Shim-pack CLC-ODS C_(18) column(150 mm×6.0 mm,5μm),the mobile phase was acetonitrile-water(38∶62,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 365 nm,the column temperature was 32℃,and the injection volume was 20μL,the flow rate of nitrogen was 2.8 L/min,the temperature of drift tube was 55℃,and the gain was 2.Results The TLC chromatograms of Aucklandiae Radix,Astragali Radix,Atractylodis Macrocephalae Rhizoma and Glycyrrhizae Radix et Rhizoma showed clear spots and good separation without interference from the negative control.The limit of detection(LOD)of aconite diester-alkaloids was 7.5μg.The mass concentration of astragalosideⅣhad a good linear relationship with the peak area in the range of 0.0241-0.3856 mg/mL(r=0.9996,n=5).The RSDs of precision,stability and repeatability tests were less than 2.3%.The average recovery of aconite diester-alkaloids was 97.35%with an RSD of 2.03%(n=9).Conclusion The quality standard established in this study is accurate and reliable,which can be used for the quality control of Anchang Liquid.