Hashimoto K, Urakami K, Fujiwara Y, Terada S, Watanabe C
Kyoto Pharmaceutical University, 5 Nakauchi-cho, Misasagi, Yamashina, Kyoto 607-8414, Japan.
Anal Sci. 2001 May;17(5):645-8. doi: 10.2116/analsci.17.645.
A novel method for the determination of residual solvents in pharmaceuticals by thermal desorption (TD)-GC/MS has been established. A programmed temperature pyrolyzer (double shot pyrolyzer) is applied for the TD. This method does not require any sample pretreatment and allows very small amounts of the sample. Directly desorbed solvents from intact pharmaceuticals (ca. 1 mg) in the desorption cup (5 mm x 3.8 mm i.d.) were cryofocused at the head of a capillary column prior to a GC/MS analysis. The desorption temperature was set at a point about 20 degrees C higher than the melting point of each sample individually, and held for 3 min. The analytical results using 7 different pharmaceuticals were in agreement with those obtained by direct injection (DI) of the solution, followed by USP XXIII. This proposed TD-GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents. Furthermore, this method was simple, allowed rapid analysis and gave good repeatability.
已建立一种通过热脱附（TD）-气相色谱/质谱联用技术测定药品中残留溶剂的新方法。采用程序升温热解器（双脉冲热解器）进行热脱附。该方法无需任何样品预处理，且允许使用极少量样品。在气相色谱/质谱分析之前，将解吸杯（内径5 mm×3.8 mm）中完整药品（约1 mg）直接解吸出的溶剂在毛细管柱柱头进行冷聚焦。解吸温度设定为比每个样品各自熔点高约20℃的点，并保持3分钟。使用7种不同药品的分析结果与通过溶液直接进样（DI）并遵循美国药典XXIII获得的结果一致。所提出的热脱附-气相色谱/质谱联用方法被证明对残留溶剂的鉴定和定量非常有用。此外，该方法操作简单，分析速度快，重复性好。
