HPLC-MS/MS法测定桑菊感冒片中5个成分的含量
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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片中芦丁、绿原酸、连翘苷、桔梗皂苷D和苦杏仁苷的含量。方法:采用Atlantis C_(18)色谱柱(2.1 mm×150 mm,5μm),以乙腈(A)-0.1%甲酸(B)为流动相,梯度洗脱(0~3 min,20%A;3~15 min,20%A→60%A;15~23 min,60%A;23~24 min,60%A→20%A;24~30 min,20%A),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质量浓度均在0.01~2μg·m L~(-1)的范围内线性关系良好(r>0.999),苦杏仁苷质量浓度在0.25~50μg·m L~(-1)的范围内线性关系良好(r>0.999),平均回收率(n=6)分别为98.9%、99.8%、100.6%、99.4%、99.6%,RSD分别为0.84%、0.90%、1.2%、1.3%、0.86%;3批样品中芦丁、绿原酸、连翘苷、桔梗皂苷D和苦杏仁苷含量范围分别为244.0~267.9、257.3~278.8、170.9~190.0、169.3~177.8、4763.9~4872.5μg·g~(-1)。结论:所建立的方法为桑菊感冒片的全面质量控制提供科学依据。
Objective:To establish a method for the determination of rutin,chlorogenic acid,forsythin,platycodin D and amygdalin in Sangju Ganmao tablets by HPLC-MS/MS.Methods:The determination was carried out on an Atlantis C_(18) column(2.1 mm×150 mm,5μm)at 35℃.The mobile phase consisted of acetonitrile(A)-0.1%formic acid solution(B)with gradient elution(0-3 min,20%A;3-15 min,20%A→60%A;15-23 min,60%A;23-24 min,60%A→20%A;24-30 min,20%A)at a flow rate of 0.2 m L·min~(-1).The analytes were detected by tandem mass spectrometry with the electrospray ionization(ESI)source combined with multiple reaction monitoring(MRM)modes.Results:Rutin,chlorogenic acid,forsythin and platycodin D showed good linearities in the range of 0.01-2μg·m L~(-1)(r>0.999).Amygdalin showed a good linearity in the range of 0.25-50μg·m L~(-1)(r>0.999).The average recoveries(n=6)were 98.9%,99.8%,100.6%,99.4%and 99.6%with RSDs of 0.84%,0.90%,1.2%,1.3%and 0.86%.The contents of rutin,chlorogenic acid,forsythin,platycodon D and amygdalin in 3 batches of samples were 244.0-267.9μg·g~(-1),257.3-278.8μg·g~(-1),170.9-190.0μg·g~(-1),169.3-177.8μg·g~(-1) and 4 763.9-4 872.5μg·g~(-1),respectively.Conclusion:This method can be used for the overall assessment of the quality of Sangju Ganmao tablets.
Objective:To establish a method for the determination of rutin,chlorogenic acid,forsythin,platycodin D and amygdalin in Sangju Ganmao tablets by HPLC-MS/MS.Methods:The determination was carried out on an Atlantis C_(18) column(2.1 mm×150 mm,5μm)at 35℃.The mobile phase consisted of acetonitrile(A)-0.1%formic acid solution(B)with gradient elution(0-3 min,20%A;3-15 min,20%A→60%A;15-23 min,60%A;23-24 min,60%A→20%A;24-30 min,20%A)at a flow rate of 0.2 m L·min~(-1).The analytes were detected by tandem mass spectrometry with the electrospray ionization(ESI)source combined with multiple reaction monitoring(MRM)modes.Results:Rutin,chlorogenic acid,forsythin and platycodin D showed good linearities in the range of 0.01-2μg·m L~(-1)(r>0.999).Amygdalin showed a good linearity in the range of 0.25-50μg·m L~(-1)(r>0.999).The average recoveries(n=6)were 98.9%,99.8%,100.6%,99.4%and 99.6%with RSDs of 0.84%,0.90%,1.2%,1.3%and 0.86%.The contents of rutin,chlorogenic acid,forsythin,platycodon D and amygdalin in 3 batches of samples were 244.0-267.9μg·g~(-1),257.3-278.8μg·g~(-1),170.9-190.0μg·g~(-1),169.3-177.8μg·g~(-1) and 4 763.9-4 872.5μg·g~(-1),respectively.Conclusion:This method can be used for the overall assessment of the quality of Sangju Ganmao tablets.
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):494ZHAO ZX,WANG M,WANG YN,et al.Simultaneous determination of five saponins in Xinkeshu capsules by UPLC-MS/MS[J].Chin J Pharm Anal,2016,36(3):494
[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):1606SHI H,ZHANG QY,YANG HT,et al.Simultaneous quantification of 8 main active constituents in Jianwei Xiaoshi tablets by liquid chromatography tandem mass spectrometry[J].Chin J Pharm Anal,2015,35(9):1606
[17]任艳平,常路,曹亮,等.HPLC-MS法同时测定舒血宁注射液中萜类内酯和黄酮醇苷的含量[J].药物分析杂志,2013,33(2):220REN YP,CHANG L,CAO L,et al.Simultaneous determination of terpene lactones and favonoid aglycones in Shuxuening injection by HPLC-MS[J].Chin J Pharm Anal,2013,33(2):220
[18]蔡晓翠,贺金华,顾政一,等.HPLC-MS/MS法同时测定新疆一枝蒿药材中5个成分的含量[J].药物分析杂志,2013,33(10):1672CAI XC,HE JH,GU ZY,et al.Simultaneous determination of 5constitunes in Aremisia rupestris L.by HPLC-MS/MS[J].Chin J Pharm Anal,2013,33(10):1672
[19]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):123ZHANG C,XING DG.Effect of platycodin D on the apoptosis of MG-63 cells[J].J Guangdong Pharm Univ,2017,33(1):123
[20]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):823ZOU XS,SHAN JJ,XIE T,et al.Advances in the study of platycodin D[J].Chin Tradit Pat Med,2014,36(4):823
[21]QU YL,ZHOU L,WANG CL.Effects of platycodin D on IL-1β-induced inflammatory response in human osteoarthritis chondrocytes[J].Int Immunopharmacol,2016,40:474
[22]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):78FANG XX,HUANG BT,ZENG JX,et al.Content difference of total saponins and platycodin-D in Platycodonis Radix from different origins[J].Chin J Exp Tradit Med Form,2016,22(1):78
[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):96YAO J,ZHANG C.Study on extraction process of Sangjuganmao mixture[J].Guide China Med,2014,12(25):96
[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):47YANG ZY.30 cases of coughing after colds in spring with Sanju changed drink[J].J North Pharm,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,2013SUN LY.Improvement of Production Process of Sangjuganmao Tablets[D].Tianjin:Tianjin University,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,2010,19(17):173WEI CY.Cold treatment of 26 cases of pregnancy Sangju decoction[J].Chin J Ethnomed Ethnopharm,2010,19(17):173
[6]中华人民共和国药典2015年版.一部[S].2015:1464,297,310,170,277,201 Ch P 2015.VolⅠ[S].2015:1464,297,310,170,277,201
[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):193MAO C,ZHENG J,ZOU YH.Content determination of chlorogenic acid,luteolin glycosides and 3,5-O-dicaffeoylquinic acid in Sangju Ganmao tablets with HPLC[J].Chin Arch Tradit Chin Med,2014,31(1):193
[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):54DING DY,GAO F,YAO L,et al.Determination of platycodin D in tablets of Sangju for common cold by HPLC-ELSD[J].Chin J Inf Tradit Chin Med,2012,19(3):54
[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):348YUAN CQ,QIU HY,KANG HY.Determination of chlorogenic acid in Sangjuganmao tablets by HPLC[J].Chin J Hosp Pharm,2010,30(4):348
[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):855LIU ZW.Content determination of forsythin and liquiritin in Sangjuganmao tablets by HPLC[J].Her Med,2008,27(7):855
[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):2379ZHANG L,HE B.Determination of the content of chlorogenic acid in Sangju Ganmao tablets by HPLC[J].Mod Med Health,2007,23(16):2379
[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):250LI J,WU ZR.Content determination of forsythin in Sangjuganmao tablets by HPLC[J].J Pract Tradit Chin Intern Med,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,2006:242LI M.Quality Control of Traditional Chinese Medicine[M].Beijing:China Medical Science Press,2006:242
[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,2006:196LI M.Market Dynamics and Application Prospect of Traditional Chinese Medicine[M].Beijing:China Medical Science Press,2006:196
[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):494ZHAO ZX,WANG M,WANG YN,et al.Simultaneous determination of five saponins in Xinkeshu capsules by UPLC-MS/MS[J].Chin J Pharm Anal,2016,36(3):494
[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):1606SHI H,ZHANG QY,YANG HT,et al.Simultaneous quantification of 8 main active constituents in Jianwei Xiaoshi tablets by liquid chromatography tandem mass spectrometry[J].Chin J Pharm Anal,2015,35(9):1606
[17]任艳平,常路,曹亮,等.HPLC-MS法同时测定舒血宁注射液中萜类内酯和黄酮醇苷的含量[J].药物分析杂志,2013,33(2):220REN YP,CHANG L,CAO L,et al.Simultaneous determination of terpene lactones and favonoid aglycones in Shuxuening injection by HPLC-MS[J].Chin J Pharm Anal,2013,33(2):220
[18]蔡晓翠,贺金华,顾政一,等.HPLC-MS/MS法同时测定新疆一枝蒿药材中5个成分的含量[J].药物分析杂志,2013,33(10):1672CAI XC,HE JH,GU ZY,et al.Simultaneous determination of 5constitunes in Aremisia rupestris L.by HPLC-MS/MS[J].Chin J Pharm Anal,2013,33(10):1672
[19]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):123ZHANG C,XING DG.Effect of platycodin D on the apoptosis of MG-63 cells[J].J Guangdong Pharm Univ,2017,33(1):123
[20]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):823ZOU XS,SHAN JJ,XIE T,et al.Advances in the study of platycodin D[J].Chin Tradit Pat Med,2014,36(4):823
[21]QU YL,ZHOU L,WANG CL.Effects of platycodin D on IL-1β-induced inflammatory response in human osteoarthritis chondrocytes[J].Int Immunopharmacol,2016,40:474
[22]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):78FANG XX,HUANG BT,ZENG JX,et al.Content difference of total saponins and platycodin-D in Platycodonis Radix from different origins[J].Chin J Exp Tradit Med Form,2016,22(1):78