高效液相色谱法测定肝胆双清口服液中3种成分含量  

Content Determination of Three Components in Gandan Shuangqing Oral Liquid

作　　者：杨国平 YANG Guoping(Nujiang Lisu Autonomous Prefecture for Food and Drug Inspection Institute,Nujiang,Yunnan,China 673199)

机构地区：[1]云南省怒江傈僳族自治州食品药品检验所,云南怒江673199

出　　处：《中国药业》2024年第15期76-80,共5页China Pharmaceuticals

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-C_(18)柱(150 mm×4.6 mm,3.5μm),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 Acclaim^(TM)120A C_(18)柱(250 mm×4.6 mm,5μm),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0.323 1~0.325 8 mg/mL、0.285 8~0.287 6 mg/mL、0.268 8~0.305 5 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。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-C_(18) 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 Acclaim^(TM) 120A C_(18) 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 RSDs of3.04%,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.

关 键 词：肝胆双清口服液 高效液相色谱法 牛磺熊去氧胆酸 牛磺鹅去氧胆酸 特女贞苷 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0