气相-热能色谱法测定药用丁基胶塞中11种N-亚硝胺及亚硝胺可生成物的提取量

Determination the extraction of 11 N-nitrosamines and N-nitrosatable substances in butyl rubber stopper by GC-TEA

目的:建立气相色谱-热能检测器法,用于测定药用丁基胶塞中11种N-亚硝胺及亚硝胺可生成物在3种介质中的提取量。方法:采用DB-FFAP色谱柱(30 m×320μm×1.0μm),通过程序升温,以N-亚硝基-双异丙基胺(NDiPA)为内标,直接提取的方法进行测试。结果:11种N-亚硝胺能达到完全分离,在2~100 ng·mL^-1或5~100 ng·mL^-1浓度范围内线性良好,检测下限和定量下限分别为0.6~4.4ng·mL^-1,1.6~15 ng·m L^-1。在pH 2.5缓冲液、pH 8.0缓冲液和甲醇中的回收率均在80%~105%之间。应用于7批丁基胶塞的检测,有1种亚硝胺被检出,均低于规定限度。结论:该方法相较于现有方法更简便、准确,灵敏度高,重复性好,适用于胶塞中N-亚硝胺提取量的测定。

Objective:To establish a GC-TEA method for the determination of 11 N-Nitrosaminesand N-nitrosatable substances in three different extraction mediaof butyl rubber stoppers.Methods:Direct determination using DB-FFAP column(30 m×320μm×1.0μm),N-nitroso-diisopropylamine(NDIPA)asthe internal standard.Results:11 N-nitrosamines were completelyseparated,the calibration curve swere linear between 2-100 ng·mL^-1 or 5-100 ng·mL^-1,the LOD and LOQ were 0.6-4.4 ng·mL^-1 and 1.6-15 ng·mL^-1 respectively,the recovery in pH 2.5 buffer,pH 8.0 buffer and methanol medium were between 80%-105%.One type of nitrosamine and N-nitrosatable substance was found from 7 batchs of butyl rubber stoppers.Conclusion:This method is simple,accurate andhas high sensitivity.It can be used for the determination of nitrosamines extraction form rubber stoppers.