HPLC-MS/MS法测定桑菊感冒丸中3种成分的含量
|
摘要
目的:建立同时测定桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的方法。方法:采用高效液相色谱-串联质谱法。色谱柱为Waters Atlantis C_(18),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.2 mL/min,柱温为35℃,进样量为10μL。离子源为电喷雾离子源,采用多反应监测扫描模式和正离子检测模式,干燥气和雾化气均为高纯氮气,干燥气温度为270℃,干燥气流量为25 L/min,鞘气流量为10 L/min,毛细管电压为4 500 V,喷嘴电压为2 000 V,扫描时间为0.1 s。结果:芦丁、连翘苷和桔梗皂苷D检测质量浓度线性范围分别为0.010 82~2.164μg/mL(r=0.999 7)、0.010 18~2.036μg/mL(r=0.999 4)、0.010 27~2.054μg/mL(r=0.999 7);定量限分别为1.250、0.260、2.720 ng/mL,检测限分别为0.380、0.078、0.820 ng/mL;精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为97.88%~99.88%(RSD=0.72%,n=6)、98.48%~103.13%(RSD=1.91%,n=6)、98.79%~101.41%(RSD=1.05%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的同时测定。
OBJECTIVE:To establish the method for simultaneous determinations of rutin,forsythin and platycodin D in Sangju ganmao pills. METHODS:HPLC-MS method was adopted. The determination was performed on Waters Atlantis C_(18) column with mobile phase consisted of acetonitrile-0.1% formic acid(gradient elution)at the flow rate of 0.2 mL/min. The column temperature was set 35 ℃,and sample size was 10 μL. The ionization mode was electrospray ion,and the reaction mode was multi-reaction monitoring. By positive ion detection mode,the drying gas and nebuliser gas were all high purity nitrogen. The drying gas temperature was 270 ℃.The drying gas flow rate was 25 L/min. The sheath gas flow rate was 10 L/min. The capillary voltage was 4 500 V. The nozzle voltage was 2 000 V and the scanning time was 0.1 s. RESULTS:The linear range of rutin,forsythin and platycodin D were 0.010 82-2.164 μg/mL(r=0.999 7),0.010 18-2.036 μg/mL(r=0.999 4),0.010 27-2.054 μg/mL(r=0.999 7),respectively. The limits of quantification were 1.250,0.260,2.720 ng/mL,and the limits of detection were 0.380,0.078,0.820 ng/mL. RSDs of precision,stability and reproducibility tests were all no more than 3.0%. The recoveries were 97.88%-99.88%(RSD=0.72%,n=6),98.48%-103.13%(RSD=1.91%,n=6),98.79%-101.41%(RSD=1.05%,n=6). CONCLUSIONS:This method is simple,precise,stable and reproducible,and can be used for simultaneous determination of rutin,forsythin and platycodin D in Sangju ganmao pills.
OBJECTIVE:To establish the method for simultaneous determinations of rutin,forsythin and platycodin D in Sangju ganmao pills. METHODS:HPLC-MS method was adopted. The determination was performed on Waters Atlantis C_(18) column with mobile phase consisted of acetonitrile-0.1% formic acid(gradient elution)at the flow rate of 0.2 mL/min. The column temperature was set 35 ℃,and sample size was 10 μL. The ionization mode was electrospray ion,and the reaction mode was multi-reaction monitoring. By positive ion detection mode,the drying gas and nebuliser gas were all high purity nitrogen. The drying gas temperature was 270 ℃.The drying gas flow rate was 25 L/min. The sheath gas flow rate was 10 L/min. The capillary voltage was 4 500 V. The nozzle voltage was 2 000 V and the scanning time was 0.1 s. RESULTS:The linear range of rutin,forsythin and platycodin D were 0.010 82-2.164 μg/mL(r=0.999 7),0.010 18-2.036 μg/mL(r=0.999 4),0.010 27-2.054 μg/mL(r=0.999 7),respectively. The limits of quantification were 1.250,0.260,2.720 ng/mL,and the limits of detection were 0.380,0.078,0.820 ng/mL. RSDs of precision,stability and reproducibility tests were all no more than 3.0%. The recoveries were 97.88%-99.88%(RSD=0.72%,n=6),98.48%-103.13%(RSD=1.91%,n=6),98.79%-101.41%(RSD=1.05%,n=6). CONCLUSIONS:This method is simple,precise,stable and reproducible,and can be used for simultaneous determination of rutin,forsythin and platycodin D in Sangju ganmao pills.
引文
[1]吴瑭.温病条辨[M].北京:中国中医药出版社,2006:90-97.
[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,2010,19(17):173.
[6]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:1463-1464.
[7]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.
[8]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.
[9]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.
[10]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):250-251.
[11]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.
[12]孙志,胡玉荣,左莉华,等.UPLC-MS/MS法同时测定复方血栓通胶囊中9种成分的含量[J].中国药房,2017,28(21):2959-2963.
[13]李霄,吴茵,支旭然,等.UPLC-MS/MS法同时测定苦黄注射液中7种成分的含量[J].中国药房,2017,28(15):2108-2112.
[14]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.
[15]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.
[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,2010,19(17):173.
[6]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:1463-1464.
[7]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.
[8]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.
[9]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.
[10]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):250-251.
[11]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.
[12]孙志,胡玉荣,左莉华,等.UPLC-MS/MS法同时测定复方血栓通胶囊中9种成分的含量[J].中国药房,2017,28(21):2959-2963.
[13]李霄,吴茵,支旭然,等.UPLC-MS/MS法同时测定苦黄注射液中7种成分的含量[J].中国药房,2017,28(15):2108-2112.
[14]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.
[15]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.