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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 establish a method for the determination of benzene solvent in capsule ink by capillary gas chromatography. Methods: The capillary column was AT-1 (30m × 0.32 mm × 0.25μm). The inlet temperature was 250 ℃, the FID detector was 250 ℃ and the column temperature was 40 ℃ for 5 min. ℃ .min-1 heating rate was raised to 200 ℃ for 3 min, the determination of benzene solvent content. Results: Under the selected chromatographic conditions, the four substances were well separated and the precision (n = 6) was 4.3% for benzene, 1.7% for toluene, 1.1% for paraxylene and 1.1% 6) were 113.6% for benzene, 120.1% for toluene, 114.9% for p-xylene and 115.3% for o-xylene respectively. The limits of detection were respectively 0.4μg.mL-1 for benzene, 0.2μg.mL-1 for toluene and 0.2μg for p- mL-1, o-xylene 0.2 μg.mL-1. After testing, the content of benzene in the samples were less than 0.4μg.mL-1, toluene, paraxylene, o-xylene content of less than 0.2μg.mL-1. Conclusion: This method was verified by preliminary methodological study and could be used for the detection of benzene-based solvents in capsule ink printing.