热重/差热分析-固相微萃取-气相色谱-质谱联用系统的建立与应用  

Establishment and Application of Combination System of Thermogravimetry/Differential Thermal Analyzer-Solid Phase Microextration-Gas Chromatography-Mass Spectrometry

作　　者：朱文辉 杨柳 杨红燕[1,2] 吴亿勤 董学畅[3] 缪明明[4] 

机构地区：[1]红塔烟草(集团)有限责任公司技术中心,玉溪653100 [2]云南大学化学科学与工程学院,昆明650091 [3]云南民族大学化学与生物技术学院,昆明650031 [4]云南烟草科学研究院,昆明650106

出　　处：《分析化学》2010年第4期527-531,共5页Chinese Journal of Analytical Chemistry

摘　　要：根据非平衡态固相微萃取理论,建立了热重/差热分析-固相微萃取-气相色谱-质谱联用系统,并按照划分温度段取样的方法,将其应用于原儿茶醛热解行为的研究,以验证联用系统的可靠性和分析方法的可行性。采用此系统,在10℃/min升温速率、200mL/min氦气流速条件下,在140～380℃温度范围内监测并分析了原儿茶醛的10种热解逸出产物的含量变化和原儿茶醛本体的迁移情况。结果表明,此联用系统在分析复杂组分逸出行为方面有明显优势;根据热解产物色谱峰面积计算得到的联用系统相对标准偏差(n=5)小于10%,证明此联用系统具有较高的可靠性,能够用于热解行为的研究。A new combination system of thermogravimetry/differential thermal analyzer-solid phase microex-tration-gas chromatography-mass spectrometry（TG/DTA-SPME-GC-MS） was designed on the basis of the adsorption theory of SPME in nonequilibrium situations.A new sampling method at different temperature ranges for TG/DTA-SPME-GC-MS was established to study the pyrolysis behavior of protocatechuic aldehyde. Identification and monitoring of the evolved behavior of 10 pyrolysis products from the pyrolysis at flowing helium of 200 mL/min and heating rate of 10℃/min and the migration of protocatechuic aldehyd was carried out between 140 and 380℃to test the combination system and verify the analytical method.Results show that TG/DTA-SPME-GC-MS has obvious advantages in the analysis of complex pyrolysis products.The combination system has high reliability and can be used for the study of pyrolysis behavior.The relative standard deviations（RSDs）（n=5） calculated from the chromatogram peak areas of pyrolytic products are all lower than 10%.

关 键 词：热重/差热分析 固相微萃取 气相色谱-质谱 热解行为 原儿茶醛 

分 类 号：O657.63[理学—分析化学]