HPLC-MS/MS法测定桑菊感冒丸中5种成分的含量
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摘要
目的建立高效液相色谱-串联质谱法同时测定桑菊感冒丸中芦丁、绿原酸、连翘苷、桔梗皂苷D和苦杏仁苷的含量。方法采用Waters Atlantis C18色谱柱(150 mm×2. 1 mm,5μm);以乙腈(A)-体积分数0. 1%甲酸(B)为流动相,梯度洗脱;流速0. 2 m L·min~(-1);柱温35℃;采用电喷雾离子源(ESI),以多反应监测(MRM)方式进行正离子扫描。结果芦丁、绿原酸、连翘苷和桔梗苷D分别在质量浓度0. 01～2 mg·L~(-1)内线性关系良好(r> 0. 999),苦杏仁苷在质量浓度0. 25～50 mg·L~(-1)内线性关系良好(r> 0. 999),平均回收率(n=6)分别为98. 82%、98. 96%、99. 43%、99. 19%和98. 88%,RSD分别为0. 7%、1. 3%、1. 4%、0. 8%和1. 1%。结论所建立的方法为桑菊感冒丸的全面质量控制提供科学依据。
Objective To establish the method for determinations of rutin,chlorogenic acid,forsythin,platycodin D and amygdalin in Sangju Ganmao Pills by HPLC-M S/M S. Methods The determination was carried out with Waters Atlantis C18column( 150 mm × 2. 1 mm,5 μm). The mobile phase consisted of acetonitrile( A)-0. 1% formic acid solution( B) with gradient elution at a flow rate of 0. 2 mL·min~(-1)at35 ℃. The analytes were detected by tandem mass spectrometry with the electrospray ionization( ESI)source combined with multiple reaction monitoring( M RM) mode. Results Rutin,chlorogenic acid,forsythin and platycodin D showed a good linearity in the range of 0. 01-2 mg·L~(-1)( r > 0. 999). The amygdalin showed a good linearity in the range of 0. 25-50 mg·L~(-1)( r > 0. 999). The average recoveries( n = 6)were 98. 82%,98. 96%,99. 43%,99. 19%,98. 88%,with the RSD were 0. 7%,1. 3%,1. 4%,0. 8%,1. 1%. Conclusion This method is reliable,accurate,which offers advantages of high sensitivity and precision. It can be used for the overall assessment of the quality of Sangju Ganmao Pills.
Objective To establish the method for determinations of rutin,chlorogenic acid,forsythin,platycodin D and amygdalin in Sangju Ganmao Pills by HPLC-M S/M S. Methods The determination was carried out with Waters Atlantis C18column( 150 mm × 2. 1 mm,5 μm). The mobile phase consisted of acetonitrile( A)-0. 1% formic acid solution( B) with gradient elution at a flow rate of 0. 2 mL·min~(-1)at35 ℃. The analytes were detected by tandem mass spectrometry with the electrospray ionization( ESI)source combined with multiple reaction monitoring( M RM) mode. Results Rutin,chlorogenic acid,forsythin and platycodin D showed a good linearity in the range of 0. 01-2 mg·L~(-1)( r > 0. 999). The amygdalin showed a good linearity in the range of 0. 25-50 mg·L~(-1)( r > 0. 999). The average recoveries( n = 6)were 98. 82%,98. 96%,99. 43%,99. 19%,98. 88%,with the RSD were 0. 7%,1. 3%,1. 4%,0. 8%,1. 1%. Conclusion This method is reliable,accurate,which offers advantages of high sensitivity and precision. It can be used for the overall assessment of the quality of Sangju Ganmao Pills.
引文
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[15]赵振霞,王敏,王钰宁,等. UPLC-MS/MS法测定心可舒胶囊中5种皂苷类成分的含量[J].药物分析杂志,2016,36(3):494-499.
[16]史贺,张巧月,杨浩天,等. HPLC-MS/MS法同时测定健胃消食片中8种化学成分的含量[J].药物分析杂志,2015,35(9):1606-1611.
[17]姚彤,金希儒,毛煦,等. HPLC-MS/MS法同时测定毛樱桃叶中7种黄酮类成分的含量[J].沈阳药科大学学报,2017,34(3):221-228.
[18]赵莹. HPLC-MS/MS法同时测定坤复康片中5种有效成分的含量[J].沈阳药科大学学报,2015,32(11):869-874.
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[20]张程,邢德刚.桔梗皂苷D对MG-63细胞的凋亡作用[J].广东药科大学学报,2017,33(1):123-126.
[21]邹葭霜,单进军,谢彤,等.桔梗皂苷D的研究进展[J].中成药,2014,36(4):823-827.
[22]QU Y L,ZHOU L,WANG C L. Effects of platycodin D on IL-1β-induced inflammatory response in human osteoarthritis chondrocytes[J]. International Immunopharmacology,2016,40:474-479.
[23]方香香,黄碧涛,曾金祥,等.不同产地桔梗药材中总皂苷及桔梗皂苷D的含量比较[J].中国实验方剂学杂志,2016,22(1):78-81.
[2]姚静,张超.桑菊感冒合剂提取工艺的研究[J].中国医药指南,2014,12(25):96-97.
[3]杨周贇.桑菊饮化裁治疗春季感冒后咳嗽30例[J].北方药学,2013,10(7):47.
[4]孙立艳.桑菊感冒片生产工艺改进[D].天津:天津大学,2013.
[5]韦春燕.桑菊饮加减治疗妊娠期感冒26例[J].中国民族民间医药,2010,17:173.
[6]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.
[7]茅纯,郑娟,邹耀华.高效液相色谱法同时测定桑菊感冒片中绿原酸、木犀草苷和3,5-O-二咖啡酰基奎宁酸含量[J].中华中医药学刊,2014,31(1):193-195.
[8]丁大勇,高菲,姚琳,等. HPLC-ELSD法测定桑菊感冒片中桔梗皂苷D的含量[J].中国中医药信息杂志,2012,19(3):54-55.
[9]袁才琼,邱海蕴,康红英.高效液相色谱法测定桑菊感冒片中绿原酸的含量[J].中国医院药学杂志,2010,30(4):348-349.
[10]刘志武.高效液相色谱法同时测定桑菊感冒片中连翘苷和甘草苷含量[J].医药导报,2008,27(7):855-856.
[11]张雷,何兵. HPLC测定桑菊感冒片中绿原酸的含量[J].现代医药卫生,2007,23(16):2379-2381.
[12]李洁,吴政然.高效液相色谱法测定桑菊感冒片中连翘苷的含量[J].实用中医内科杂志,2006,20(3):250.
[13]李敏.中药材质量与控制[M].北京:中国医药科技出版社,2006:242-244.
[14]李敏.中药材市场动态及应用前景[M].北京:中国医药科技出版社,2006:196-200.
[15]赵振霞,王敏,王钰宁,等. UPLC-MS/MS法测定心可舒胶囊中5种皂苷类成分的含量[J].药物分析杂志,2016,36(3):494-499.
[16]史贺,张巧月,杨浩天,等. HPLC-MS/MS法同时测定健胃消食片中8种化学成分的含量[J].药物分析杂志,2015,35(9):1606-1611.
[17]姚彤,金希儒,毛煦,等. HPLC-MS/MS法同时测定毛樱桃叶中7种黄酮类成分的含量[J].沈阳药科大学学报,2017,34(3):221-228.
[18]赵莹. HPLC-MS/MS法同时测定坤复康片中5种有效成分的含量[J].沈阳药科大学学报,2015,32(11):869-874.
[19]张稀雯.桑菊感冒颗粒的制备工艺及质量标准研究[D].武汉:武汉理工大学,2012.
[20]张程,邢德刚.桔梗皂苷D对MG-63细胞的凋亡作用[J].广东药科大学学报,2017,33(1):123-126.
[21]邹葭霜,单进军,谢彤,等.桔梗皂苷D的研究进展[J].中成药,2014,36(4):823-827.
[22]QU Y L,ZHOU L,WANG C L. Effects of platycodin D on IL-1β-induced inflammatory response in human osteoarthritis chondrocytes[J]. International Immunopharmacology,2016,40:474-479.
[23]方香香,黄碧涛,曾金祥,等.不同产地桔梗药材中总皂苷及桔梗皂苷D的含量比较[J].中国实验方剂学杂志,2016,22(1):78-81.