HPLC法同时测定清肺抑火片中5种游离蒽醌类和5种结合蒽醌类成分含量
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摘要
目的建立同时测定清肺抑火片中5种游离蒽醌类和5种结合蒽醌类成分含量的HPLC-UV方法。方法采用Phenomenex Luna C18(250 mm×4. 6 mm,5μm)色谱柱,以甲醇(A)-体积分数0. 1%磷酸水(B)为流动相,梯度洗脱,流速为1. 0 m L·min~(-1),检测波长为254 nm,柱温为25℃。结果芦荟大黄素-8-O-葡萄糖苷、大黄酸-8-O-β-D-葡萄糖苷、大黄酚-8-O-β-D-葡萄糖苷、大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-β-D-葡萄糖苷,以及芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚分别在质量浓度2. 13～170. 40 mg·L~(-1)、1. 12～89. 60 mg·L~(-1)、0. 43～34. 12 mg·L~(-1)、0. 54～43. 60mg·L~(-1)、1. 50～120. 40 mg·L~(-1)、0. 94～74. 80 mg·L~(-1)、0. 67～53. 60 mg·L~(-1)、0. 36～28. 92 mg·L~(-1)、1. 29～103. 20 mg·L~(-1)和1. 09～87. 20 mg·L~(-1)内线性关系良好;精密度、重复性试验结果 RSD值均小于3%;样品在24 h内峰面积RSD均小于3%;各成分加样回收率均在95%～105%内,RSD均小于3%。结论该方法可为完善清肺抑火片的质量标准提供依据。
Objective To establish a method for the simultaneous determination of 5 kinds of free anthraquinone and 5 kinds of combined anthraquinone in Qingfeiyihuo Tablets by HPLC-UV. Methods The chromatographic column was Phenomenex Luna C18( 250 mm × 4. 6 mm,5 μm) column,and the flow phase was methanol( A)-0. 1% phosphate water( B) by gradient elute. The flow rate was 1. 0 mL·min~(-1),detection wavelength was at 254 nm,and column temperature was 25 ℃. Results Aloe-emodin-8-Oglucopyranoside, rhein-8-O-glucopyranoside, chryohol-8-O-β-D-glucoyroide, emodin-8-O-glucoside,physcion-8-O-β-D-monoglucoside,aloe-emodin,rhein,emodin,chrysophanol and physcion had good linear relations among 2. 13~(-1)70. 40 mg·L~(-1),1. 12-89. 60 mg·L~(-1),0. 43-34. 12 mg·L~(-1),0. 54-43. 60 mg·L~(-1),1. 50~(-1)20. 40 mg·L~(-1),0. 94-74. 80 mg·L~(-1),0. 67-53. 60 mg·L~(-1),0. 36-28. 92 mg·L~(-1),1. 29~(-1)03. 20 mg·L~(-1)and 1. 09-87. 20 mg·L~(-1). The RSD of each component peak area was less than 3% in precision test. The RSD of the content of the repeated test was less than 3% in repetitive test.The RSD of the sample in 24 h was less than 3%. The recovery rate of each component was between 95%and 105%,and the RSD was less than 3%. Conclusion The method is easy to operate,have characteristics of rapid analysis and high accuracy,which can provide a basis for the improvement of the quality standard of Qingfeiyihuo Tablets.
Objective To establish a method for the simultaneous determination of 5 kinds of free anthraquinone and 5 kinds of combined anthraquinone in Qingfeiyihuo Tablets by HPLC-UV. Methods The chromatographic column was Phenomenex Luna C18( 250 mm × 4. 6 mm,5 μm) column,and the flow phase was methanol( A)-0. 1% phosphate water( B) by gradient elute. The flow rate was 1. 0 mL·min~(-1),detection wavelength was at 254 nm,and column temperature was 25 ℃. Results Aloe-emodin-8-Oglucopyranoside, rhein-8-O-glucopyranoside, chryohol-8-O-β-D-glucoyroide, emodin-8-O-glucoside,physcion-8-O-β-D-monoglucoside,aloe-emodin,rhein,emodin,chrysophanol and physcion had good linear relations among 2. 13~(-1)70. 40 mg·L~(-1),1. 12-89. 60 mg·L~(-1),0. 43-34. 12 mg·L~(-1),0. 54-43. 60 mg·L~(-1),1. 50~(-1)20. 40 mg·L~(-1),0. 94-74. 80 mg·L~(-1),0. 67-53. 60 mg·L~(-1),0. 36-28. 92 mg·L~(-1),1. 29~(-1)03. 20 mg·L~(-1)and 1. 09-87. 20 mg·L~(-1). The RSD of each component peak area was less than 3% in precision test. The RSD of the content of the repeated test was less than 3% in repetitive test.The RSD of the sample in 24 h was less than 3%. The recovery rate of each component was between 95%and 105%,and the RSD was less than 3%. Conclusion The method is easy to operate,have characteristics of rapid analysis and high accuracy,which can provide a basis for the improvement of the quality standard of Qingfeiyihuo Tablets.
引文
[1]林瑞群,姚五湖. HPLC法测定清肺抑火片中栀子苷的含量[J].中药新药与临床药理,2009,20(2):161-162.
[2]李海霞,杨辉,徐远金,等.毛细管电泳-质谱联用法测定清肺抑火片中的四种有效成分[J].分析科学学报,2012,28(1):43-47.
[3]周浓,杨勤,于杰,等.高效液相色谱法测定不同厂家清肺抑火片中黄芩苷的含量[J].西南大学学报:自然科学版,2012,34(9):153-156.
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[5]付艳芬,王剑华,周浓,等. HPLC法测定不同厂家清肺抑火片中5种蒽醌类衍生物的含量[J].中国药房,2012,23(12):1136-1139.
[6]叶秀金,宋粉云. HPLC法测定清肺抑火丸中大黄的四种成分的含量[J].中药新药与临床药理,2010,21(6):646-648.
[7]汪霞. RP-HPLC法同时测定清肺抑火片中大黄3种成分的含量[J].中国药事,2008,22(1):49-51.
[8]马志英.高效液相色谱-双波长紫外检测同时测定清肺抑火片中4种药效成分[J].中成药,2012,34(12):2330-2334.
[9]邵维在,段治尚,万德生,等.清肺抑火片质量标准研究[J].大理大学学报,2017,2(2):20-23.
[10]张村,李丽,肖永庆,等.大黄5种饮片中游离蒽醌类成分比较研究[J].中国中药杂志,2009,34(15):1914-1916.
[11]王芳,王珍珍,茅向军,等.土大黄游离蒽醌类成分HPLC指纹图谱[J].中国实验方剂学杂志,2017,23(8):72-76.
[12]乌仁图雅,萨日盖,萨茹拉,等.不同产地民族药材大黄中蒽醌类成分的含量对比研究[J].中国民族医药杂志,2017,23(6):41-42.
[13]李棣华,刘俊红,伍孝先.一种提高大黄饮片中结合型蒽醌的原药材炮制方法研究[J].天津中医药,2014,31(6):373-375.
[14]冯素香,王哲,郝蕊,等. HPLC法同时测定不同产地掌叶大黄中10个蒽醌类化合物[J].药物分析杂志,2017,37(5):783-788.
[15]曲毅,王伽伯,李会芳,等.蒽醌类中药的致泻强度与化学含量相关性研究[J].中国中药杂志,2008,33(7):806-808.
[2]李海霞,杨辉,徐远金,等.毛细管电泳-质谱联用法测定清肺抑火片中的四种有效成分[J].分析科学学报,2012,28(1):43-47.
[3]周浓,杨勤,于杰,等.高效液相色谱法测定不同厂家清肺抑火片中黄芩苷的含量[J].西南大学学报:自然科学版,2012,34(9):153-156.
[4]国家药典委员会.中华人民共和国药典:一部[M].北京:中国医药科技出版社,2015:1540-1541.
[5]付艳芬,王剑华,周浓,等. HPLC法测定不同厂家清肺抑火片中5种蒽醌类衍生物的含量[J].中国药房,2012,23(12):1136-1139.
[6]叶秀金,宋粉云. HPLC法测定清肺抑火丸中大黄的四种成分的含量[J].中药新药与临床药理,2010,21(6):646-648.
[7]汪霞. RP-HPLC法同时测定清肺抑火片中大黄3种成分的含量[J].中国药事,2008,22(1):49-51.
[8]马志英.高效液相色谱-双波长紫外检测同时测定清肺抑火片中4种药效成分[J].中成药,2012,34(12):2330-2334.
[9]邵维在,段治尚,万德生,等.清肺抑火片质量标准研究[J].大理大学学报,2017,2(2):20-23.
[10]张村,李丽,肖永庆,等.大黄5种饮片中游离蒽醌类成分比较研究[J].中国中药杂志,2009,34(15):1914-1916.
[11]王芳,王珍珍,茅向军,等.土大黄游离蒽醌类成分HPLC指纹图谱[J].中国实验方剂学杂志,2017,23(8):72-76.
[12]乌仁图雅,萨日盖,萨茹拉,等.不同产地民族药材大黄中蒽醌类成分的含量对比研究[J].中国民族医药杂志,2017,23(6):41-42.
[13]李棣华,刘俊红,伍孝先.一种提高大黄饮片中结合型蒽醌的原药材炮制方法研究[J].天津中医药,2014,31(6):373-375.
[14]冯素香,王哲,郝蕊,等. HPLC法同时测定不同产地掌叶大黄中10个蒽醌类化合物[J].药物分析杂志,2017,37(5):783-788.
[15]曲毅,王伽伯,李会芳,等.蒽醌类中药的致泻强度与化学含量相关性研究[J].中国中药杂志,2008,33(7):806-808.