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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 qualitative and quantitative analysis of related substances in 1,1,1,2-tetrafluoroethane by GC-MS and GC. Methods: The GC chromatographic conditions were as follows: DB-1301 (120 m × 0.25 mm × 1 μm) column was used. The carrier gas was high purity nitrogen. The inlet temperature was 200 ℃ and the flow rate was 1 mL · min- The temperature of the column was controlled by programmed temperature (-20 ° C for 12 min, temperature raised to 190 ° C at 10.0 ° C · min-1 for 5 min, cooled with liquid nitrogen). The GC part of the GC-MS condition is the same as above. Under the condition of mass spectrometry, the carrier gas is high-purity helium, 70 eV, EI ion source, and the mass scanning range is 40 to 400 amu. Results: The gas chromatogram and the corresponding mass spectrum of the related substances were obtained. The corresponding substances were identified as 2-chloro-1,1,1-trifluoroethane, 2-chloro-1,1,1-trifluoroethane, -1,1,1,2-tetrafluoropropane, 2-chloro-1,1-difluoroethylene, 1,2-dichloro-1,1,2,2-tetrafluoroethane, 1,1-bis Chloro-1,2,2,2-tetrafluoroethane, chlorodifluoromethane, 1,1,2,2-tetrafluoroethane, 1,1,1-trifluoropropene, 1,1,1- Trifluoroethane, 1,1-difluoroethane, chloropentafluoroethane, pentafluoroethane, and chlorofluoroethylene. Conclusion: This study provides a scientific basis for the study of drug safety and product quality of 1,1,1,2-tetrafluoroethane.