【摘要】 建立了超声提取/气相色谱-质谱(GC-MS)联用法检测红树林沉积物中蒲公英萜醇的方法,对仪器测试、提取、皂化、衍生化、数据处理等多个参数进行了优化,保证了方法的有效性和实用性。选用HP-5MS毛细色谱柱快速分离测定红树林沉积物中的蒲公英萜醇,根据标准物质的保留时间、主要特征离子及其相对丰度和平均质谱图定性;在选择离子监测(SIM)模式下,根据蒲公英萜醇和内标衍生物定量离子的峰面积比值,以内标标准曲线法定量。实验结果表明,在5~100μg/L范围内,衍生物定量离子峰面积比值与蒲公英萜醇浓度呈良好的线性关系,相关系数为0.999,方法的定量下限为0.5μg/kg。当加标水平为5~80μg/L时,回收率为81.2%~108.3%,相对标准偏差(RSD)为1.9%~4.2%。本方法具有良好的选择性、灵敏度,适用于红树林沉积物中蒲公英萜醇的测定,并成功应用于实际样品的分析,可为红树林海岸带的保护和管理提供技术支持。更多还原

【Abstract】 A gas chromatography- mass spectrometric method with ultrasonic extraction was developed for the determination of taraxerol in mangrove sediments. The parameters including instrument condition,extraction,saponification,derivatization and data analysis were optimized. The analyte was separated by GC with an HB- 5MS capillary column,then identified and quantified by the characteristic chromatograms properties and retention time. The component was separated completely from others,simultaneously identified and quantified with the standard curves. Quantitation using internal standard was based on the ratio of peak area of taraxerol derivative to peak area of internal standard derivative in the selected ion monitoring mode with electron impact source. The calibration curve was linear in the range of 5- 100 μg / L,with a limit of quantitation of 0. 5 μg / kg. The mean recoveries at 5,20,80 μg / L spiked levels were in the range of 81. 2%- 108. 3%,with relative standard deviations of 1. 9%- 4. 2%. The results showed that the developed method was sensitive,accurate and reproducible,and was suitable for the analysis of taraxerol in mangrove sediments. The study could provide scientific evidences for the management and protection of mangrove.更多还原