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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 gas chromatography method for the determination of three related substances, aniline, 2-aminophenol and 4-aminophenol in mesalazine enteric-coated tablets. Method: The carrier gas was high purity nitrogen (99.999%) and the flow rate was 15 m L · min-1 using an Agilent HP-5 (5% Ph Me Silicone) capillary column (10 m × 0.53 mm × 2.65 μm) The temperature was 280 ℃ and the FID was 300 ℃. The temperature of the column was controlled by programmed temperature (initial temperature was 70 ℃, kept for 2 min, temperature was raised to 150 ℃ at 10 ℃ · min-1 for 6 min). Results: Under the selected chromatographic conditions, the three impurities of aniline, 2-aminophenol and 4-aminophenol were well separated and the recoveries were between 97% and 103%. The precision and linear regression were good. The content of aniline in the three batches of samples was 0.00012%, the content of 2-aminophenol was 0.00022%, 0.00018% and 0.00019% respectively, and the content of 4-aminophenol was 0.00025%, 0.00024% and 0.00024% respectively. Conclusion: This method can be used for the quality control of mesalazine enteric-coated tablets.