摘要
目的 建立测定肝胆双清口服液中牛磺熊去氧胆酸、牛磺鹅去氧胆酸和特女贞苷含量的高效液相色谱法.方法 牛磺熊去氧胆酸和牛磺鹅去氧胆酸的含量测定,色谱柱为Agilent Extend-C18 柱(150 mm×4.6 mm,3.5 μm),流动相为 0.02 mol/L磷酸二氢钠溶液(用三乙胺调pH至 6.0)-乙腈(梯度洗脱),流速为 1 mL/min,检测波长为 205 nm,柱温为 40℃,进样量为 10µL;特女贞苷的含量测定,色谱柱为Thermo AcclaimTM 120A C18 柱(250 mm×4.6 mm,5 μm),流动相为乙腈-水(梯度洗脱),流速为 1 mL/min,检测波长为 224 nm,柱温为 40℃,进样量为 10µL.结果 牛磺熊去氧胆酸、牛磺鹅去氧胆酸和特女贞苷的质量浓度分别在 0.040 0～1.000 5 mg/mL、0.031 0～0.776 0 mg/mL、0.029 3～0.731 5 mg/mL范围内与峰面积线性关系良好(r=0.999 9,n=6);精密度、稳定性、重复性试验结果的RSD均小于 2.0%(n=6);加样回收率分别为 98.49%,99.49%,99.78%,RSD分别为 3.04%,2.20%,1.15%(n=6).3批样品中3种成分的含量分别为0.3231～0.3258 mg/mL、0.2858～0.2876 mg/mL、0.2688～0.3055 mg/mL.结论 所建立的方法操作简便快速、重复性好、结果准确,可用于肝胆双清口服液中牛磺熊去氧胆酸、牛磺鹅去氧胆酸和特女贞苷的含量测定.
Abstract
Objective To establish a high-performance liquid chromatography(HPLC)method for the content determination of tauroursodeoxycholic acid,taurochenodeoxycholic acid,and specnuezhenide in Gandan Shuangqing Oral Liquid.Methods For the content determination of tauroursodeoxycholic acid and taurochenodeoxycholic acid,the chromatographic column was Agilent Extend-C18 column(150 mm×4.6 mm,3.5 mm),the mobile phase was 0.02 mol/L sodium dihydrogen phosphate aqueous solution(pH was to adjusted 6.0 with triethylamine)-acetonitrile(gradient elution),the flow rate was 1 mL/min,the detection wavelength was 205 nm,the column temperature was 40℃,and the injection volume was 10 µL.For the content determination of specnuezhenide,the chromatographic column was Thermo AcclaimTM 120A C18 column(250 mm×4.6 mm,5 mm),the mobile phase was acetonitrile-water(gradient elution),the flow rate was 1 mL/min,the detection wavelength was 224 nm,the column temperature was 40℃,and the injection volume was 10 µL.Results The linear ranges of tauroursodeoxycholic acid,aurochenodeoxycholic acid,and specnuezhenide were 0.040 0-1.000 5 mg/mL,0.031 0-0.776 0 mg/mL,and 0.029 3-0.731 5 mg/mL(r=0.999 9,n=6).The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n=6).The average recoveries of tauroursodeoxycholic acid,aurochenodeoxycholic acid,and specnuezhenide were 98.49%,99.49%,99.78%,with RSDsof 3.04%,2.20%,and 1.15%(n=6),respectively.The contents of three components in the three batches of samples were in the ranges of 0.323 1-0.325 8 mg/mL,0.285 8-0.287 6 mg/mL,and 0.268 8-0.305 5 mg/mL,respectively.Conclusion The established method is simple,quick,reproducible,and accurate,which can be used for the content determination of tauroursodeoxycholic acid,taurochenodeoxycholic acid,and specnuezhenide in Gandan Shuangqing Oral Liquid.
维普
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