UPLC-QQQMS测定咳特灵中小叶榕干浸膏12种成分

Quantification of Twelve Constituents in the Extracts of Folium ficim icrocarpae by Ultra-performence Liquid Chromatography-Quadropole Mass Spectrometry

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 Foliurn ficirn icrocarpae. The extracts were extracted with 10% CH3CN by ultrasonic extraction. The extracts were analyzed in multiple- reaction monitoring mode with an ultra-performance liquid chromatography-tandem mass spectrometry equipped with electrospray ionization and an Agilent ZORBAX HSS T3 column（2.1 mm× 100 mm, 1.8 μm）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 of quantification for all of the twelve analytes were less than 1.694 μg/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.