气相色谱法测定美沙拉嗪肠溶片中苯胺、2-氨基苯酚、4-氨基苯酚3种有关物质的含量

GC determination of aniline,2-aminophenol and 4-aminophenol in mesalazine enteric-coated tablets

目的：建立气相色谱法测定美沙拉嗪肠溶片中苯胺、2-氨基苯酚、4-氨基苯酚3种有关物质的含量。方法：采用安捷伦HP-5（5%Ph Me Silicone）毛细管柱（10 m×0.53 mm×2.65μm）,载气为高纯氮气（99.999%）,流速15 m L·min-1,进样口温度280℃,氢火焰离子检测器（FID）300℃,柱温为程序升温（起始温度70℃,保持2 min,以10℃·min-1的速率升温至150℃,维持6 min）。结果：在选定的色谱条件下,苯胺、2-氨基苯酚、4-氨基苯酚3个杂质分离度良好,回收率在97%∽103%之间,精密度、线性回归等良好。3批样品中苯胺含量均为0.00012%;2-氨基苯酚含量分别为0.00022%、0.00018%和0.00019%;4-氨基苯酚含量分别为0.00025%、0.00024%和0.00024%。结论：本方法能用于美沙拉嗪肠溶片的质量检测。

Objective：To establish a GC method for the determination of three related substances--aniline,2-ami- nophenol and 4-aminophenol in mesalamine enteric-coated tablets. Methods：An HP-5 （5% Ph Me Silicone） 10 m×0.53 mm ×2. 65μm capillary GC column was adopted. The carrier gas was high pure nitrogen（99. 999% ） at a flow rate of 15 mL· min-1. The inlet temperature was controlled at 280 ℃ and the FID detector temperature was 300 ℃. The oven temperature was initially held at 70 ℃ for 2 min and was then programmed to 150 ℃ at the rate of 10 ℃. min -1 and held for 6 min. Results：A good resolution was obtained among the peaks of the 3 impuri- ties at these chromatographic conditions. The recoveries of aniline ,2-aminophenol and 4-aminophenol were between 97% -103%. The precision and linearity equations were good. The aniline content in the three samples were O. 00012% ,0. 00012% and 0. 00012%. The 2 -aminophenol content in the three samples were 0. 00022% , 0. 00018% and 0. 00019% ;The 4-aminophenol content in the three samples were 0. 00025% ,0. 00024% and 0. 00024%. Conclusion：The method can be used for quality test of mesalazine enteric-coated tablets.