胶囊壳油墨印字中苯类溶剂残留检测

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(30 m×0.32 mm×0.25 μm),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0.4 μg·mL^-1、甲苯0.2 μg·mL^-1、对二甲苯0.2 μg·mL^-1、邻二甲苯0.2 μg·mL^-1。经检测,样品中苯含量均小于0.4 μg·mL^-1,甲苯、对二甲苯、邻二甲苯含量均小于0.2 μg·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.

1 Determination of volatile organic compands in cigarette carton and packet packaging paper-Headspace gas chromatography(卷烟条与盒包装纸中挥发性有机化合物的测定——顶空气相色谱法).YC/T 207-2006.2007
2 Determination of benzene,toluene,xylene and toluene diisocyanates in solvent coatings-headspace-GC-MS method(溶剂型涂料中苯、甲苯、二甲苯和甲苯二异氰酸酯的测定——顶空GC-MS法).SN/T2251-2009.2010
3 SUN Wen-tong(孙文通),HUANG Zhen(黄蓁),QIU Ye(邱烨),et al.Determination of oxygenates,benzene and toluene in gasoline by GC/MS(气质联用仪测定汽油中含氧化合物、苯和甲苯的).J Chin Mass Spec Society(质谱学报),2010,31(1):59
4 Technical requirement for environmental labeling products-Gravure and flexible printing ink(环境标志产品技术要求——凹印油墨和柔印油墨).HJ/T 371-2007.2008
5 USP34/NF29.2011.467
6 ChP(中国药典).2010.Vol Ⅱ(二部):Appendix(附录)ⅧP