GC-MS法测定预灌封注射器中UV胶的挥发性成分

GC-MS determination of volatile substances in UV adhesives of prefilled syringe

目的:建立预灌封注射器中UV胶挥发性成分的分析方法。方法:采用Rtx-5M(5%二苯基-95%二甲基聚硅氧烷)毛细管色谱柱以程序升温方式顶空进样气相色谱-质谱联用方法对预灌封注射器中UV胶挥发性成分进行分析,利用对照品定位结合NIST谱库准确检定出四氢糠醇、环己酮、苯甲醛、甲基丙烯酸羟丙酯、甲基丙烯酸氢糠酯、甲基丙烯酸异冰片酯共6种物质,并利用标准曲线法对其进行定量分析。结果:6种挥发性成分均能很好分离,线性良好、检出限低、平均回收率在95%~105%范围内、RSD≤5%。预灌封注射器中UV胶挥发性成分均未检出,但在UV胶阳性样品中6种成分均有检出。结论:本法操作简便、准确、灵敏度高,可用于高风险注射剂包装预灌封注射器中UV胶挥发性成分的测定。

Objective:To establish a method for the determination of volatile substances in UV adhesives of Prefilled Syringe.Method:The volatile substances in UV adhesives of Prefilled Syringe were determined by headspace gas chromatography mass spectrometry with Rtx-5M capillary column(5%diphenyl-95%dimethylsiloxane)under the programmed temperature.Tetrahydrofurfuryl alcohol,Cyclohexanone,Benzaldehyde,2-Hydroxypropyl methacrylate,Tetrahydrofurfuryl methacrylate and Isobornyl methacrylate were identified by the retention time of reference substance combined with NIST library searching of GC-MS and were quantitatively analyzed by calibration curve method.Results:Six volatile substances were separated completely and were detected in the positive sample.But the volatile substances of UV adhesives were not detected in the Prefilled Syringe.The calibration curve of each solvent showed a good linear relationship.The limits of detection were lower,and the average recoveries were within 95%-105%with the relative standard deviations not more than 5%.Conclusion:The established method for determination of volatile substances in UV adhesives of Prefilled Syringe is simple,sensive and accurate.It is suitable for determination of volatile substances in UV adhesives of high-risk injection packaging of prefilled syringe.