HPLC-DAD法同时测定柴黄片中6种成分的含量
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篇名: HPLC-DAD法同时测定柴黄片中6种成分的含量
TITLE:
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(pH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5 μL。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 6 μg(r均≥0.999 3),检测限分别为0.008、0.007、0.005、0.005、0.020、0.018 μg/mL,定量限分别为0.025、0.022、0.015、0.015、0.060、0.054 μg/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 mL/min. The detection wavelengths were set at 210 nm (saikosaponin a, saikosaponin d) and 277 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 μg/mL. The limits of quantitation were 0.025, 0.022, 0.015, 0.015, 0.060, 0.054 μg/mL. RSDs of precision, reproducibility and stability tests (48 h) were all lower than 1.5% (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.
期刊: 2019年第30卷第11期
作者: 丁长玲,崔俊凤,石效荣,徐洋洋,成文娜,张金杰,赵丽
AUTHORS: DING Changling,CUI Junfeng,SHI Xiaorong,XU Yangyang,CHENG Wenna,ZHANG Jinjie,ZHAO Li
关键字: 高效液相色谱-二极管阵列检测器法;柴黄片;含量测定;黄芩苷;汉黄芩苷;黄芩素;汉黄芩素;柴胡皂苷a;柴胡皂苷d
KEYWORDS: HPLC-DAD; Chaihuang tablets; Content determination; Baicalin; Wogonoside; Baicalein; Wogonin; Saikosaponin a; Saikosaponin d
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