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HPLC-DAD法同时测定柴黄片中6种成分的含量

Simultaneous Determination of 6 Components in Chaihuang Tablets by HPLC-DAD

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【作者】 丁长玲崔俊凤石效荣徐洋洋成文娜张金杰赵丽

【Author】 DING Changling;CUI Junfeng;SHI Xiaorong;XU Yangyang;CHENG Wenna;ZHANG Jinjie;ZHAO Li;Dept.of Pharmacy,the Affiliated Hospital of Binzhou Medical College;Binzhou Center for Food and Drug Control;Dept.of Pain,the Affiliated Hospital of Binzhou Medical College;

【机构】 滨州医学院附属医院药学部滨州市食品药品检验检测中心滨州医学院附属医院疼痛科

【摘要】 目的:建立同时测定柴黄片中6种成分黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、柴胡皂苷a和柴胡皂苷d含量的方法。方法:采用高效液相色谱-二极管阵列检测器(HPLC-DAD)法检测同一厂家的3批柴黄片。色谱柱为Agilent Eclipse XDB-C18;流动相为乙腈-磷酸三乙胺水溶液(p H调至7.0),梯度洗脱;流速为1.0 mL/min;检测波长为210 nm(柴胡皂苷a、柴胡皂苷d)和277 nm(黄芩苷、汉黄芩苷、黄芩素、汉黄芩素);柱温为30℃;进样量为5μL。结果:黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、柴胡皂苷a和柴胡皂苷d检测进样量线性范围分别为0.379 5~7.590 4、0.082 96~1.659 2、0.039 39~0.787 8、0.040 72~0.814 4、0.040 45~0.809 0、0.038 63~0.772 6μg(r均≥0.999 3),检测限分别为0.008、0.007、0.005、0.005、0.020、0.018μg/mL,定量限分别为0.025、0.022、0.015、0.015、0.060、0.054μg/mL,精密度、重复性和稳定性试验(48 h)中的RSD<1.5%(n=6),平均加样回收率分别为98.46%、97.06%、100.90%、96.13%、96.91%、96.57%(RSD<2.0%,n=6)。结论:建立的同时测定柴黄片中6种成分含量的方法操作简便、结果准确、重复性好,可用于该制剂的质量控制。

【Abstract】 OBJECTIVE:To establish a method for simultaneous determination of 6 components in Chaihuang tablets,such as baicalin,wogonoside,baicalein,wogonin,saikosaponin a and saikosaponin d in Chaihuang tablets. METHODS:HPLC-DAD method was used to detect 3 batches of Chaihuang tablets from same manufacturers. The determination was performed on Agilent Eclipse XDB-C18 column with mobile phase consisted of acetonitrile-triethylamine phosphate aqueous solution(pH adjusted to 7.0,gradient elution)at flow rate of 1.0 m L/min. The detection wavelengths were set at 210 nm(saikosaponin a,saikosaponin d)and277 nm(baicalin,wogonoside,baicalein,wogonin). The column temperature was 30 ℃,and sample size was 5 μL. RESULTS:The linear ranges of baicalin,wogonoside,baicalein,wogonin,saikosaponin a and saikosaponin d were 0.379 5-7.590 4 μg,0.082 96-1.659 2 μg,0.039 39-0.787 8 μg,0.040 72-0.814 4 μg,0.040 45-0.809 0 μg,0.038 63-0.772 6 μg(all r≥0.999 3),respectively. The limits of detection were 0.008,0.007,0.005,0.005,0.020 and 0.018 μ g/mL. The limits of quantitation were0.025,0.022,0.015,0.015,0.060,0.054 μg/mL. RSDs of precision,reproducibility and stability tests(48 h)were all lower than1.5%(n=6). Average recoveries were 98.46%,97.06%,100.90%,96.13%,96.91%,96.57%(RSD<2.0%,n=6).CONCLUSIONS:Established method is simple,accurate and reproducible for 6 components in Chaihuang tablets,and can be used for quality control of the tablet.

【基金】 山东省自然科学基金资助项目(No.ZR2014HP067,ZR2018PH044)
  • 【分类号】R286.0
  • 【被引频次】4
  • 【下载频次】267
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