UPLC-QQQMS测定咳特灵中小叶榕干浸膏12种成分
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摘要
本文建立了超高效液相-串联四极杆质谱多反应监测模式法,同时测定小叶榕干浸膏12种成分的含量。小叶榕干浸膏提取物用体积分数为10%的乙腈溶液超声提取,提取液用安捷伦ZORBAX HSS T3色谱柱(2.1mm×100mm,1.8μm)分离,甲醇-0.1%甲酸(体积比)梯度洗脱,电喷雾电离源多反应模式监测。所建立的方法对小叶榕干浸膏12种成分的定量限均小于1.694μg/L,在定量范围内离子的色谱面积与成分质量浓度呈线性关系,相关系数均大于0.99,加样回收率为82.2%~109.5%,日内及日间精密度RSD分别为1.0%~6.0%和1.5%~5.1%。检测结果表明小叶榕干浸膏中黄酮类化合物异牡荆素、荭草素、异荭草素、芦丁含量均较高,酚类化合物奎宁酸、没食子酸含量较高。该法为进一步研究和修订咳特灵制剂的质量标准提供了科学依据。
An ultra-performance liquid chromatography-quadropole mass method was established to simultaneously quantify twelve constituents in the extracts of Folium ficim icrocarpae.The extracts were extracted with 10% CH_3CN by ultrasonic extraction.The extracts were analyzed in multiplereaction monitoring mode with an ultra-performance liquid chromatography-tandem mass spectrometry equipped with electrospray ionization and an Agilent ZORBAX HSS T3 column(2.1mm×100mm,1.8μm)using gradient MeOH-0.1% formic acid water as mobile phase.The area of the analytes showed good linearity with respect to the analyte concentrations(R2≥0.99).The limits ofquantification for all of the twelve analytes were less than 1.694μg/L and the recovery rates of the method were 82.2%~109.5%.The inter-day and intra-day relative standard deviations were 1.0%~6.0% and 1.5%~5.1%,respectively.The results showed that the extracts contained large amounts of quinic acid,gallic acid,isovitexin,vitexin,orientin,isoorientin constituents.The established method could be used asscientific evidence for the revision of the quality control of Keteling preparation.
An ultra-performance liquid chromatography-quadropole mass method was established to simultaneously quantify twelve constituents in the extracts of Folium ficim icrocarpae.The extracts were extracted with 10% CH_3CN by ultrasonic extraction.The extracts were analyzed in multiplereaction monitoring mode with an ultra-performance liquid chromatography-tandem mass spectrometry equipped with electrospray ionization and an Agilent ZORBAX HSS T3 column(2.1mm×100mm,1.8μm)using gradient MeOH-0.1% formic acid water as mobile phase.The area of the analytes showed good linearity with respect to the analyte concentrations(R2≥0.99).The limits ofquantification for all of the twelve analytes were less than 1.694μg/L and the recovery rates of the method were 82.2%~109.5%.The inter-day and intra-day relative standard deviations were 1.0%~6.0% and 1.5%~5.1%,respectively.The results showed that the extracts contained large amounts of quinic acid,gallic acid,isovitexin,vitexin,orientin,isoorientin constituents.The established method could be used asscientific evidence for the revision of the quality control of Keteling preparation.
引文
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[2]国家药典委员会.中华人民共和国药典一部[M].2015版.北京:中国医药科技出版社,2015:1182-1183.
[3]郭亚健,范莉,王晓强,等.关于NaNO2-Al(NO3)3-NaOH比色法测定总黄酮方法的探讨[J].药物分析杂志,2002,22(2):97-98.
[4]贾茹冰.咳特灵胶囊中小榕树膏总黄酮的含量测定[J].广西中医学院学报,2000,17(4):65-66.
[5]赖毅勤,刘峰,周宏兵,等.小叶榕叶水提物浸膏的HPLC指纹图谱初步研究[J].广东药学院学报,2008,24(1):6-8.
[6]员荣,孙丽丽,管淑玉,等.小叶榕干浸膏及咳特灵胶囊的HPLC指纹图谱研究及LC-Q-TOF-MS成分分析[J].中国实验方剂学杂志,2016,22(3):6-8.
[7]刘力恒,王立升,王天文,等.小叶榕叶总黄酮含量测定、鉴别及其对羟基自由基清除作用的研究[J].时珍国医国药,2008,19(5):1078-1080.
[8]陈化,陈明颖,梁斌.高效液相色谱法测定小叶榕浸膏中牡荆素的含量[J].中国药师,2008,11(7):749-750.
[9]陈路,蓝鸣生,李永玺.小叶榕浸膏质量标准研究[J].时珍国医国药,2009,20(1):78-79.
[10]陈如意,罗培,李怡杰,等.HPLC测定四方藤中3种岩白菜素类化合物的含量[J].广西师范大学学报(自然科学版),2015,33(1):99-103.
[11]丘琴,甄汉深,陈明伟,等.壮药龙利叶茎HPLC指纹图谱研究[J].广西师范大学学报(自然科学版),2016,34(2):116-121.
[12]CHENG H,LIN C,LIN T.Antiherpes simplex virus type2activity of casuarinin from the bark of Terminalia arjuna Linn[J].Antiviral Res,2002,55(3):447-55.