高效液相色谱法同时测定藏药六味丁香散中4种成分的含量
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摘要
目的建立高效液相色谱法同时测定藏药六味丁香散中4种成分的含量。方法采用高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂(250 mm×4.6 mm,5μm),以乙腈为流动相A,以0.05%磷酸溶液为流动相B,梯度洗脱,流速1 mL·min~(-1),检测波长268 nm,柱温30℃,进样量为10μL。结果没食子酸、土木香内酯、异土木香内酯、丁香酚线性范围分别为0.415～2.490μg·mL~(-1)(r=0.9999)、0.026～0.255μg·mL~(-1)(r=0.9999)、0.028～0.275μg·mL~(-1)(r=0.9999)、0.560～3.360μg·mL~(-1)(r=0.9999);精密度、稳定性、重复性试验均符合方法学测定要求;平均回收率分别在99.2%～101.1%、98.4%～100.0%、98.6%～101.0%、101.2%～101.6%,RSD值均<2.0%(n=3)。结论本方法准确、简便,可用于藏药六味丁香散中4种成分含量的同时测定。
Objective To establish an HPLC method to simultaneously determine 4 effective components in Tibetan medicine Liuwei Dingxiang pulvis. Methods C18 column(250 mm×4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile(A) and 0.05% phosphori cacid aqueous solution(B) with gradient elution at the flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃, the detection wavelength was 268 nm, and the injection volume was 10 μL. Results The linear ranges of gallic acid, alantolactone, isoalantolactone, and eugenol were 0.415-2.490 μg·mL~(-1)(r = 0.9999), 0.026-0.255 μg·m L~(-1)(r = 0.9999), 0.028-0.275 μg·mL~(-1)(r = 0.9999), and 0.560-3.360 μg·mL~(-1)(r = 0.9999). The method was precise, stable and repeatable, meeting the requirements of methodology. The average recovery was 99.2%-101.1%, 98.4%-100.0%, 98.6%-101.0%, and 101.2%-101.6%, and the RSD value were less than 2.0%. Conclusion This method is accurate and simple. It can be used to control the quality of Liuwei Dingxiang pulvis.
Objective To establish an HPLC method to simultaneously determine 4 effective components in Tibetan medicine Liuwei Dingxiang pulvis. Methods C18 column(250 mm×4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile(A) and 0.05% phosphori cacid aqueous solution(B) with gradient elution at the flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃, the detection wavelength was 268 nm, and the injection volume was 10 μL. Results The linear ranges of gallic acid, alantolactone, isoalantolactone, and eugenol were 0.415-2.490 μg·mL~(-1)(r = 0.9999), 0.026-0.255 μg·m L~(-1)(r = 0.9999), 0.028-0.275 μg·mL~(-1)(r = 0.9999), and 0.560-3.360 μg·mL~(-1)(r = 0.9999). The method was precise, stable and repeatable, meeting the requirements of methodology. The average recovery was 99.2%-101.1%, 98.4%-100.0%, 98.6%-101.0%, and 101.2%-101.6%, and the RSD value were less than 2.0%. Conclusion This method is accurate and simple. It can be used to control the quality of Liuwei Dingxiang pulvis.
引文
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[8]杨凤梅. GC法测定六味丁香丸中丁香酚的含量[J].青海医药杂志,2007,37(8):92-94.
[9]杨洋,黄良永,朱美玲,等.一测多评法中中国药典2015年版中的应用[J].中南药学,2017,15(12):1742-1745.
[10]逯雯洁,王慧春,海平,等.高效液相色谱法同时测定二十五味珍珠丸中7种成分及其特征图谱[J].中国医院药学杂志,2016,36(21):1885-1890.
[11]冯欣,鲁晓光,罗布扎西,等. HPLC法同时测定藏药七味铁屑丸中木香烃内酯和去氢木香内酯[J].中成药,2011,33(9):1535-1538.
[12]倪玲,杨锡. HPLC法同时测定达斯玛保丸中木香烃内酯、异土木香内酯和土木香内酯[J].中国药房,2012,34(4):664-667.
[2]卫生部药品标准(藏药第一册)[S].北京:化学工业出版社,1995:98.
[3]陈发奎.中药有效成分含量测定[M].北京:人民卫生出版社,2008:259.
[4]肖远灿,胡凤祖. RP-HPLC测定藏木香中土木香内酯和异土木香内酯含量[J].中国药学杂志,2007,42(7):491-493.
[5]李先端,顾雪竹,肖碧英,等.绒毛诃子与诃子质量评价与比较[J].中国实验方剂学杂志,2010,16(17):48-52.
[6]罗光伟,陈建江.诃子的药理作用研究进展[J].云南中医中药杂志,2012,33(11):78-80.
[7]余小平.高效液相色谱法测定丁香中丁香酚的含量[J].药物分析杂志,2008,28(6):975-977.
[8]杨凤梅. GC法测定六味丁香丸中丁香酚的含量[J].青海医药杂志,2007,37(8):92-94.
[9]杨洋,黄良永,朱美玲,等.一测多评法中中国药典2015年版中的应用[J].中南药学,2017,15(12):1742-1745.
[10]逯雯洁,王慧春,海平,等.高效液相色谱法同时测定二十五味珍珠丸中7种成分及其特征图谱[J].中国医院药学杂志,2016,36(21):1885-1890.
[11]冯欣,鲁晓光,罗布扎西,等. HPLC法同时测定藏药七味铁屑丸中木香烃内酯和去氢木香内酯[J].中成药,2011,33(9):1535-1538.
[12]倪玲,杨锡. HPLC法同时测定达斯玛保丸中木香烃内酯、异土木香内酯和土木香内酯[J].中国药房,2012,34(4):664-667.