1,1,1,2-四氟乙烷中有关物质的气相色谱和质谱联用分析

GC and GC- MS analysis of 1,1,1,2- tetrafluoroethane and its related substances

目的:用GC-MS和GC法对1,1,1,2-四氟乙烷中的有关物质进行定性、定量分析。方法:GC色谱条件,采用DB-1301(120 m×0.25 mm×1μm)色谱柱,载气为高纯氮气,进样口温度200℃,流速1 mL·min-1,FID检测器温度180℃,柱温为程序升温(-20℃保持12 min,以10.0℃·min-1速率升温到190℃,保持5 min,液氮冷却)。GC-MS条件的GC部分同上,质谱条件,载气为高纯氦气,70 eV,EI离子源,质量扫描范围为40～400 amu。结果:得到了有关物质的气相色谱图及相应的质谱图,对其进行解析,初步鉴定出各有关物质为2-氯-1,1,1-三氟乙烷;氟氯甲烷;2-氯-1,1,1,2-四氟丙烷;2-氯-1,1-二氟乙烯;1,2-二氯-1,1,2,2-四氟乙烷;1,1-二氯-1,2,2,2-四氟乙烷;一氯二氟甲烷;1,1,2,2-四氟乙烷;1,1,1-三氟丙烯;1,1,1-三氟乙烷;1,1-二氟乙烷;氯五氟乙烷;五氟乙烷;氯氟乙烯。结论:为研究1,1,1,2-四氟乙烷用药安全及提高产品质量提供了科学依据。

Objective： To identify and quantify the related substances in 1,1,1,2- tetrafluoroethane by GC-MS and GC. Methods： The GC conditions were optimized as follows：DB-1301 capillary column （120 m×0.25 mm×1.0 μm）, high purity nitrogen as carrier gas,injector temperature was 200℃,and the flow rate was 1 mL·min-1,FID detector temperature was 180℃,column temperature was kept at -20℃ for 12 min,then rose to 190℃ at a rate of 10℃·min-1 and maintained for 5 min. Liquid nitrogen was used for cooling down.The GC-MS conditions were as follows：High purity helium as carrier gas with electronic ionization EI,70 eV,ms scanning was set at the range of 40-400 amu. Results： The total GC chromatogram and mass spectra of each chromatographic peak were obtained and analyzed,the related substance HCFC-133a,HCFC-31,HCFC-124,HCFC-1122,CFC-114,CFC-114a,HCFC-22,HFC-134,HFC-1243zf,HFC-143a,HFC-152a,CFC-115,HFC-125,HCFC-1131a were identified. Conclusion： The present study provides a scientific basis for the medication safety analysis and quality improvement of 1,1,1,2- tetrafluoroethane.