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目的以静态顶空装置模拟工作场所环境,以气相色谱质谱联用技术对毒物进行分离定性,建立现场毒物快速识别的方法。以全蒸发顶空气相色谱质谱联用技术建立化工原料中挥发性有机化合物的快速定量检测方法。方法采用静态顶空装置,对34种常见挥发性有机溶剂进行气化,组分经DB-5MS毛细管色谱柱分离后依次进入质谱检测器,以保留时间和特征离子进行定性检测。以全蒸发顶空气相色谱质谱联用对34种有机化合进行标准曲线绘制。结果 34种挥发性有机化合物能达到较好分离,根据保留时间和特征离子定性准确度高,库检索匹配度均>95%。34种有机化合物在相应的线性范围内线性良好,相关系数均>0.995,且方法重现性好,低、中、高浓度6次检测结果的相对标准偏差为1.17%~5.0%。结论该方法快速、简单、科学地模拟了工作场所环境,气相色谱质谱联用技术能对复杂样品进行有效分离和准确定性,可用于现场毒物快速识别,同时应用全蒸发顶空气色谱质谱联用法可快速定量测定化工原料中各挥发性有机化合物的含量。
Objective To simulate the workplace environment with static headspace devices and to separate and characterize the poisons by gas chromatography-mass spectrometry (GC-MS) technology to establish a rapid identification method of poison in the field. A Rapid and Quantitative Determination Method of Volatile Organic Compounds in Chemical Materials by Pervaporation Headspace Gas Chromatography-Mass Spectrometry. Methods The static headspace device was used to gasify 34 kinds of common volatile organic solvents. The components were separated by DB-5MS capillary column and then entered the mass spectrometer detector sequentially. The retention time and characteristic ions were used for qualitative detection. The 34 organic compounds were subjected to standard curve by headspace gas chromatography-mass spectrometry. Results 34 kinds of volatile organic compounds could be separated well. According to the retention time and the high qualitative accuracy of the characteristic ions, the library retrieval matching degree was> 95%. All the 34 organic compounds showed good linearity in the corresponding linear range with the correlation coefficients> 0.995. The reproducibility of the method was good. The relative standard deviations (RSDs) of the six test results were 1.17% -5.0%. Conclusion The proposed method can simulate the workplace environment quickly, easily and scientifically. Gas chromatography-mass spectrometry (GC-MS / MS) can effectively separate and characterize complex samples and can be used for rapid identification of poison in the field. Simultaneously, headspace gas chromatography-mass spectrometry Rapid and quantitative determination of volatile organic compounds in chemical raw materials.