HPLC-DAD法同时测定柴黄片中6种成分的含量
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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。
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-C_(18) 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.
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-C_(18) 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.
引文
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[5]陈翔,张红萍,许景景.HPLC法同时测定化痰平喘片中黄芩苷、黄芩素和汉黄芩素的含量[J].中国药房,2016,27(6):846-848.
[6]魏晓萌,严华,陆以云,等.HPLC法同时测定锥叶柴胡中6个主要皂苷类成分的含量[J].药物分析杂志,2018,38(4):618-622.
[7]王慧竹,王肃樊,邓博文,等.HPLC法同时测定清肺抑火丸中9种成分的含量[J].中药材,2018,41(3):652-656.
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[10]胡丹.HPLC-QAMS同时测定复方黄芩片中6种活性成分的含量[J].中国药房,2018,29(11):1510-1514.
[11]王冬梅,高靥,张洪霞,等.HPLC法同时测定芩连片中黄芩苷、黄芩素和汉黄芩素的含量[J].沈阳药科大学学报,2011,28(12):955-958.
[12]郝乘仪,郭淑英,朱鹤云,等.HPLC法同时测定牛黄清感胶囊中6个成分的含量[J].药物分析杂志,2017,37(3):422-426.
[13]刘来正,冀小君,堐榜琴.HPLC法同时测定黑柴胡药材中柴胡皂苷a和d的含量[J].中国药房,2014,25(23):2147-2149.
[14]赵佳文,瞿领航,刘艳菊,等.多成分含量测定结合UPLC指纹图谱及其模式判别评价子芩与枯芩质量[J].中药材,2017,40(9):2101-2106.
[15]吉晓丽.黄芩的化学成分与药理作用研究进展[J].中医临床研究,2017,9(9):128-129.
[16]辛国,赵昕彤,黄晓巍.柴胡化学成分及药理作用研究进展[J].吉林中医药,2018,38(10):1196-1198.
[17]李丽莉,吕轶峰,朱雪妍.葛根芩连片多成分含量测定的研究[J].药物分析杂志,2017,37(9):1607-1614.
[2]李军,姜华,张延萍,等.HPLC测定柴黄片中柴胡皂苷b1、b2的含量[J].中国药学杂志,2011,46(1):61-63.
[3]李恩泽,刘月芬,刘玉君,等.不同产地黄芩中6种化学成分含量测定[J].中国医院药学杂志,2018,38(9):49-51.
[4]刘玉梅,周安,俞年军,等.HPLC-DAD双波长法同时测定柴胡中5种皂苷的含量[J].中国中药杂志,2018,43(2):363-368.
[5]陈翔,张红萍,许景景.HPLC法同时测定化痰平喘片中黄芩苷、黄芩素和汉黄芩素的含量[J].中国药房,2016,27(6):846-848.
[6]魏晓萌,严华,陆以云,等.HPLC法同时测定锥叶柴胡中6个主要皂苷类成分的含量[J].药物分析杂志,2018,38(4):618-622.
[7]王慧竹,王肃樊,邓博文,等.HPLC法同时测定清肺抑火丸中9种成分的含量[J].中药材,2018,41(3):652-656.
[8]孟杰,陈兴福,杨文钰,等.柴胡主根与侧根中柴胡皂苷a及皂苷d含量测定[J].药物分析杂志,2013,33(7):1218-1222.
[9]卫昊,刘清,卫伟光,等.HPLC法测定秦岭柴胡及其不同提取物中柴胡皂苷a和柴胡皂苷d[J].中成药,2013,35(2):342-345.
[10]胡丹.HPLC-QAMS同时测定复方黄芩片中6种活性成分的含量[J].中国药房,2018,29(11):1510-1514.
[11]王冬梅,高靥,张洪霞,等.HPLC法同时测定芩连片中黄芩苷、黄芩素和汉黄芩素的含量[J].沈阳药科大学学报,2011,28(12):955-958.
[12]郝乘仪,郭淑英,朱鹤云,等.HPLC法同时测定牛黄清感胶囊中6个成分的含量[J].药物分析杂志,2017,37(3):422-426.
[13]刘来正,冀小君,堐榜琴.HPLC法同时测定黑柴胡药材中柴胡皂苷a和d的含量[J].中国药房,2014,25(23):2147-2149.
[14]赵佳文,瞿领航,刘艳菊,等.多成分含量测定结合UPLC指纹图谱及其模式判别评价子芩与枯芩质量[J].中药材,2017,40(9):2101-2106.
[15]吉晓丽.黄芩的化学成分与药理作用研究进展[J].中医临床研究,2017,9(9):128-129.
[16]辛国,赵昕彤,黄晓巍.柴胡化学成分及药理作用研究进展[J].吉林中医药,2018,38(10):1196-1198.
[17]李丽莉,吕轶峰,朱雪妍.葛根芩连片多成分含量测定的研究[J].药物分析杂志,2017,37(9):1607-1614.