摘要
利用气相色谱-串联质谱仪的选择反应监测(SRM)模式,对卤化丁基橡胶塞、橡胶活塞、聚异戊二烯橡胶护帽、硅橡胶医疗器械等多种医用橡胶弹性体中的N-亚硝胺类物质进行检测。样品以超声极限浸提法提取,浸取液采用亚硝胺专用净化管净化。建立的方法可以实现12种N-亚硝胺及1种N-亚硝胺内标的良好分离。12种N-亚硝胺类物质在0.6~200.0 ng/mL范围内线性良好,线性相关系数在0.9993~0.9999之间,检出限范围为0.08~4.0 ng/g,定量限范围为0.4~20.0 ng/g。精密度为1.45%~7.28%(n=6)之间,加标回收率为93%~120%。该方法灵敏度高,特异性强。采用此方法对49批次医用橡胶弹性体进行检测,发现多种N-亚硝胺物质有不同程度的检出,说明医用橡胶弹性体中存在一定程度的亚硝胺残留风险。
The multiple reaction monitoring(SRM) mode of dissolution precipitation-gas chromatography-tandem mass spectrometry(GC-MS/MS) was used to detect N-nitrosamines in various medical rubber elastomers,such as halo butyl rubber stoppers,rubber pistons,polyisoprene rubber protective caps,silicone rubber medical devices.The established method can achieve good separation of 12 kinds of N-nitrosamines and 1 kind of internal standard of N-nitrosamines.The linear ranges for 12 kinds of N-nitrosamines were 0.6-200.0 ng/mL,with the correlation coefficients in the range of 0.9993-0.9999.The limits of detection were 0.08-4 ng/g,and the limits of quantification were 0.4-20.0 ng/g.The relative standard deviations were 1.45%-7.28%(n=6),and the recoveries were 93%-120%(n=3).The established exhausted extraction method by ultrasonic with nitrosamine purification tube treatment greatly simplified the sample pretreatment process,and also improved the sensitivity.This method was applied to the determination of 12 targets in 49 medical rubber elastomers.Several kinds of N-nitrosamines were detected in the samples,indicating that there was residual risk of N-nitrosamines in medical rubber elastomers.
作者
刘爱娟
刘雪婷
薄晓文
孟凯
亓晓庆
沈永
LIU Aijuan;LIU Xueting;BO Xiaowen;MENG Kai;QI Xiaoqing;SHEN Yong(Shandong Quality Inspection Center for Medical Devices,Jinan 250101;Shandong Key Laboratory of Biological Evaluation for Medical Devices,Jinan 250101;NMPA Key Laboratory for Quality Control of Pharmaceutical Packaging Materials,Jinan 250101)
出处
《分析科学学报》
CAS
CSCD
北大核心
2021年第6期783-788,共6页
Journal of Analytical Science
基金
山东省医疗器械产品质量检验中心课题(No.ZX201907)。
关键词
N-亚硝胺
医用橡胶弹性体
硅橡胶医疗器械
极限浸提
N-nitrosamines
Medical use rubber elastomer
Silicon rubber medical devices
Exhausted extraction
