摘要
目的:建立胶囊油墨印字中苯类溶剂的毛细管气相色谱测定方法。方法:采用毛细管气相色谱法,色谱柱为AT-1(30m×0.32 mm×0.25μm),进样口温度为250℃,FID检测器250℃,柱温为40℃,保持5 min,以10℃.min-1的升温速度升至200℃保持3 min,测定苯类溶剂的含量。结果:在选定的色谱条件下,4种物质分离良好,精密度(n=6)分别为苯4.3%、甲苯1.7%、对二甲苯1.1%、邻二甲苯1.1%;回收率(n=6)分别为苯113.6%、甲苯120.1%、对二甲苯114.9%、邻二甲苯115.3%;检出限分别为苯0.4μg.mL-1、甲苯0.2μg.mL-1、对二甲苯0.2μg.mL-1、邻二甲苯0.2μg.mL-1。经检测,样品中苯含量均小于0.4μg.mL-1,甲苯、对二甲苯、邻二甲苯含量均小于0.2μg.mL-1。结论:该方法经初步方法学考察证实,可用于胶囊油墨印字中苯类溶剂的检测。
Objective：To develop a gas chromatography method for determination of benzene solvents in printing ink of gelatin capsules.Methods：The analysis was carried out on an AT-1 capillary gas chromatogram column（30 m×0.32 mm×0.25 μm） with a FID detector.The temperature of injection port and detector were both 250 ℃.The temperature of the column was maintained at 40 ℃ for 5 minutes,then the temperature was raised at a rate of 10 ℃·min-1 until 200 ℃ and kept for 3 minutes.Results：A good resolution was obtained between the peaks due to benzene,methylbenzene,1,4-dimethylbenzene,and 1,2-dimethylbenzene.The precisions（n=6） were 4.3%,1.7%,1.1%,1.1% for benzene,methylbenzene,1,4-dimethylbenzene,1,2-dimethylbenzene;The average recoveries（n=6） were 113.6%,120.1%,114.9%,and 115.3%,respectively;The limits of detection were 0.4 μg·mL-1,0.2 μg·mL-1,0.2 μg·mL-1,and 0.2 μg·mL-1,respectively.The contents of benzene in samples were less than 0.4 μg·mL-1.The contents of methylbenzene,1,4-dimethylbenzene,and 1,2-dimethylbenzene in samples were less than 0.2 μg·mL-1.Conclusion：This established method can be applied to examine benzene,methylbenzene,1,4-dimethylbenzene,and 1,2-dimethylbenzene in printing ink of gelatin capsules.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2012年第8期1325-1327,1356,共4页
Chinese Journal of Pharmaceutical Analysis
关键词
药用胶囊
油墨
溶剂残留
苯
甲苯
对二甲苯
邻二甲苯
毛细管气相色谱法
药用辅料安全监测
gelatin capsules
printing ink
residue solvents
benzene
methylbenzene
1
4-dimethylbenzene
1
2-dimethylbenzene
capillary gas chromatography
pharmaceutical excipients safety monitoring
