HPLC法测定通关藤药材中2种皂苷含量
|
摘要
目的建立测定通关藤药材中通关藤苷A和I含量的方法。方法通关藤粉末经甲醇溶解超声后,用高效液相色谱法(HPLC)进样分析,用Symmetry C18(250 mm×4.6 mm,5μm)色谱柱,乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱(0~10 min,32%A;10~15 min,42%A;15~28 min,50%A);检测波长:223nm;流速:1 mL·min~(-1)。考察方法的专属性、标准曲线、精度度、加样回收率、稳定性、重现性。结果通关藤苷A的线性范围为47.2~225.0μg·mL~(-1);低、中、高3个质量浓度平均加样回收率分别为98.82%,99.24%,99.20%。通关藤苷I的线性范围为10.5~50.0μg·mL~(-1),低、中、高3个质量浓度平均加样回收率分别为98.53%,98.32%,98.70%。通关藤药材中通关藤苷A含量为5.81~5.96 mg·g~(-1),通关藤苷I含量为0.68~0.71 mg·g~(-1)。结论该方法准确、简便、可靠,可为通关藤药材质量控制提供参考。
Objective To develop an HPLC method for determination of the proportion of tenacissoside A and I in Marsdeniatenacissima.Methods Marsdeniatenacissima powder was dissoluted by methanol,treated by ultrasonic,analyzed by HPLC,using Symmetry C_(18) column( 250 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile-0. 1%phosphoric water,gradient elution( 0~(-1)0 min,32% A; 10~(-1)5 min,42% A; 15-28 min,50% A). The flow rate was 1 mL · min~(-1). The detection wavelength was 223 nm. The specificity,standard curve,accuracy,sample recovery,stability and reproducibility of the method were investigated. Results The calibration curves of tenacissoside A were linear in the rangesof 47. 2-225. 0 μg·mL~(-1). The average recoveries of three concentrations tenacissoside A were 98. 82%,99. 24%,99. 20%respectively. The calibration curves of tenacissoside I were linear in the ranges of 10. 5-50. 0 μg · mL~(-1). The average recoveries of three concentrations tenacissoside I were 98. 53%,98. 32%,98. 70% respectively. The content of tenacissoside A was 5. 81-5. 96 mg·g~(-1). The content of tenacissoside I was 0. 68-0. 71 mg ·g~(-1). Conclusion The established method is accurate,simple and reliable,which can be used for the quality concrol of Marsdeniatenacissima.
Objective To develop an HPLC method for determination of the proportion of tenacissoside A and I in Marsdeniatenacissima.Methods Marsdeniatenacissima powder was dissoluted by methanol,treated by ultrasonic,analyzed by HPLC,using Symmetry C_(18) column( 250 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile-0. 1%phosphoric water,gradient elution( 0~(-1)0 min,32% A; 10~(-1)5 min,42% A; 15-28 min,50% A). The flow rate was 1 mL · min~(-1). The detection wavelength was 223 nm. The specificity,standard curve,accuracy,sample recovery,stability and reproducibility of the method were investigated. Results The calibration curves of tenacissoside A were linear in the rangesof 47. 2-225. 0 μg·mL~(-1). The average recoveries of three concentrations tenacissoside A were 98. 82%,99. 24%,99. 20%respectively. The calibration curves of tenacissoside I were linear in the ranges of 10. 5-50. 0 μg · mL~(-1). The average recoveries of three concentrations tenacissoside I were 98. 53%,98. 32%,98. 70% respectively. The content of tenacissoside A was 5. 81-5. 96 mg·g~(-1). The content of tenacissoside I was 0. 68-0. 71 mg ·g~(-1). Conclusion The established method is accurate,simple and reliable,which can be used for the quality concrol of Marsdeniatenacissima.
引文
[1]国家药典委员会.中华人民共和国药典(四部)[S].北京:中国医药科技出版社,2015:296-297.
[2]方奕奇,孙雪梅.通关藤化学成分及抗肿瘤作用的研究进展[J].中国生化药物杂志,2011,32(2):165-167.
[3]韩丽,张慧,康廷国,等.中药通关藤的研究进展[J].中华中医药学刊,2016,34(10):2329-23317.
[4]张贵君.现代中药材商品通鉴[M].北京:中国中医药出版社,2001:1200.
[5]白爽,李奕诺,徐鑫,等.通关藤化学成分及药理活性研究进展[J].解放军药学学报,2015,31(3):260.
[6]谢丽艳,徐洁,戴国梁,等.HPLC同时测定消癌平注射液中7种主要成分的含量[J].中国实验方剂学杂志,2013,19(21):86-89.
[7]张阿琴,张仓,梁敬钰.HPLC法测定消癌平注射液中5种酚酸的含量[J].药学与临床研究,2011,19(6):498-500.
[2]方奕奇,孙雪梅.通关藤化学成分及抗肿瘤作用的研究进展[J].中国生化药物杂志,2011,32(2):165-167.
[3]韩丽,张慧,康廷国,等.中药通关藤的研究进展[J].中华中医药学刊,2016,34(10):2329-23317.
[4]张贵君.现代中药材商品通鉴[M].北京:中国中医药出版社,2001:1200.
[5]白爽,李奕诺,徐鑫,等.通关藤化学成分及药理活性研究进展[J].解放军药学学报,2015,31(3):260.
[6]谢丽艳,徐洁,戴国梁,等.HPLC同时测定消癌平注射液中7种主要成分的含量[J].中国实验方剂学杂志,2013,19(21):86-89.
[7]张阿琴,张仓,梁敬钰.HPLC法测定消癌平注射液中5种酚酸的含量[J].药学与临床研究,2011,19(6):498-500.