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目的:利用中等极性色谱系统建立一套完整的残留溶剂定性分析体系。方法:采用DB-624色谱柱(6%氰丙基苯基-94%二甲基聚硅氧烷,0.32 mm×30 m×1.8μm),柱温40℃,维持8 min,以8℃·min-1升至120℃,维持15 min。氢火焰离子化检测器(FID),检测器温度为250℃,进样口温度为200℃,顶空温度为90℃,顶空时间为30 min;进样针温度为100℃;传输线温度110℃,载气为氮气,流速为2.0 m L·min-1,分流比为5∶1。以N-甲基吡咯烷酮为溶剂,分别对52种残留溶剂进行定性分析,测定了各残留溶剂的相对调整保留时间。结果:中等极性色谱系统与非极性色谱系统和极性色谱系统的互补性均较好,可鉴别52种残留溶剂。结论:本文建立的分析系统为完善中国药典残留溶剂定性分析提供了方法。
OBJECTIVE: To establish a complete set of qualitative analysis system for residual solvents by using medium polarity chromatographic system. Methods: DB-624 column (6% cyanopropyl phenyl-94% dimethylpolysiloxane, 0.32 mm × 30 μm × 1.8 μm) was used. The column temperature was kept at 40 ℃ for 8 min. min-1 to 120 ° C for 15 min. Flame ionization detector (FID) with detector temperature of 250 ° C, inlet temperature of 200 ° C, headspace temperature of 90 ° C, headspace time of 30 min, needle temperature of 100 ° C, and transmission line temperature of 110 ° C ℃, the carrier gas is nitrogen, the flow rate of 2.0 m L · min-1, split ratio of 5: 1. With N-methylpyrrolidone as solvent, 52 kinds of residual solvents were qualitatively analyzed respectively, and the relative adjusted retention time of each residual solvent was determined. Results: The complementarity between the medium polar chromatographic system and the non-polar chromatographic system and the polar chromatographic system were good, and 52 kinds of residual solvents could be identified. Conclusion: The analytical system established in this paper provides a method to improve the qualitative analysis of residual solvents in Chinese Pharmacopoeia.