利用中等极性气相色谱系统分析药物残留溶剂

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×1.8 μm),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 mL·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 analysis system of residual solvents using the medium polar gas chromatography system. Methods: The analysis was carried on a column of DB-624(6% cyanopropylphenyl-94%dimethylpolysiloxane,0.32 mm×30 m×1.8 μm),the column temperature was maintained at 40 ℃ for 8 minutes,then raised at a rate of 8 ℃ per minute to 120 ℃ and maintained at 120 ℃ for 15 min.The hydrogen flame ionization detector(FID)was used with the temperatures for the injection port and the detector maintained at 200 ℃ and 250 ℃,respectively.The headspace equilibration temperature was 90 ℃ for 30 minutes,the syring temperature was 100 ℃,the transfer-line temperature was 110 ℃.The carrier gas was nitrogen with a liner velocity of about 2.0 mL per minute,and a split ratio of 5:1. N-methyl-2-pyrrolidone was used as the solvent.The 52 kinds of residual solvents were identified respectively,and the relative adjusted retention time(RART)of each residual solvent was detected. Results: The medium polar system showed good complementarity to both polar and non-polar systems,and the 52 kinds of residual solvents were identified. Conclusion: The analysis system established in this paper improved the detect method of residual solvents in Chinese Pharmacopoeia.

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