气相色谱-质谱联用法测定杜仲叶中活性成分肉桂酸

Determination of the Active Ingredient Cinnamic Acid in Eucommia Ulmoides Leaves by Gas Chromatography-Mass Spectrometry

肉桂酸作为一种安全性高的活性物质,广泛用于香精、医药以及塑料、树脂等精细化工产品中。对杜仲叶进行预处理,通过优化净化条件,利用气相色谱-质谱联用法对中草药杜仲叶中的活性物质肉桂酸的含量进行了准确地定量。结果表明,色谱柱采用Agilent HP-5 MS毛细管柱(30 m×0.25 mm×0.25μm);载气为纯度为99.999%的高纯氦气;流速为1.0 mL/min;进样口温度280℃;分流比为1∶50(体积比);利用多反应监测模式(MRM)采集样品的质谱信息,方法检出限约为0.02 mg/g,定量限为0.07 mg/g,肉桂酸在3个加标浓度下的回收率为80.2%~104.6%。开发的检测方法重现性好、回收率高、精密度高,可为中药中活性成分的准确定量提供方法参考。

As a safe active substance,cinnamic acid is widely used in flavors,medicines,and fine chemical products such as plastics and resins.Eucommia ulmoides leaves were pretreated,and the content of the active substance cinnamic acid in Chinese herbal medicine Eucommia ulmoides leaves was accurately quantified by gas chromatography-mass spectrometry by optimizing the purification conditions.The results showed that the column adopts Agilent HP-5 MS capillary column(30 m×0.25 mm×0.25μm);the carrier gas was high-purity helium with a purity of 99.999%;the flow rate was 1.0 mL/min;the inlet temperature was 280℃;the split ratio was 1∶50(volume ratio);the mass spectrometry information of the sample was collected by the multiple reaction monitoring modes(MRM),the detection limit of the method was about 0.02 mg/g,and the quantification limit was 0.07 mg/g.The recoveries at the three spiked concentrations were 80.2%~104.6%.The detection method developed has good reproducibility,high recovery rate,and high precision,which can provide a method reference for the accurate quantification of active components in traditional Chinese medicine.