固相萃取净化及超高效液相色谱-串联质谱法测定橡胶制品中的13种N-亚硝胺  

Determination of N-nitrosamines in rubber products by solid phase extraction purification and ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：陈婷[1,2] 温裕云[3,2] 欧延 弓振斌[1,2] 

机构地区：[1]厦门大学近海海洋环境国家重点实验室,福建厦门361102 [2]厦门大学环境与生态学院,福建厦门361102 [3]福建远东技术服务有限公司,福建泉州362006

出　　处：《色谱》2014年第1期89-94,共6页Chinese Journal of Chromatography

基　　金：泉州市科技项目(2012FZ17)

摘　　要：建立了固相萃取（SPE）净化、超高效液相色谱-串联质谱（UHPLc—MS／MS）测定橡胶制品中13种N-亚硝胺的方法。样品于密闭萃取瓶中于60℃下用甲醇超声萃取30min，C18固相萃取小柱对萃取液进行净化，经C18色谱柱分离，最后用电喷雾正离子（ESI＋）和多重反应监测模式（MRM）对13种N-亚硝胺进行定性、定量测定。实验中对样品前处理、色谱分离条件和质谱检测条件进行了优化。在优化的实验条件下，橡胶样品中添加N-亚硝基二甲胺（NDMA）与N-亚硝基-二乙基胺（NDEA）为500μg／kg、其他组分均为50μg／kg时，各组分的相对标准偏差（RSD，n=7）小于10％；在实际样品中的加标回收率为70．7％-117．0％；方法的检出限（LOD，以10倍标准偏差计）为0．5～500μg／kg。方法可应用于橡胶制品中13种N-亚硝胺的测定。A method using C13 solid phase extraction （SPE） for purification and ultra high per- formance liquid chromatography （UHPLC） coupled with electrospray ionization tandem mass spectrometry （ESI-MS/MS） for detection was developed to simultaneously determine 13 N- nitrosamines in rubber products. The analytes were extracted with methanol （60 ℃, 30 min） with the aid of ultrasonic technique and then purified by a C13 SPE cartridge. The analytes were separated on a C,8 chromatographic column and qualitatively and quantitatively detected by a mass spectrometer with positive ESI at multiple reaction monitoring （MRM） mode. The operat- ing parameters for UHPLC separation and ESI-MS/MS detection were also optimized. Under optimum operating conditions, the relative standard deviations （RSDs, n = 7 ） were less than 10% at spiked level of 50μg/kg for all analytes except Nonitrosodimethylamine （NDMA） and N-nitrosodiethylamine （NDEA） which were spiked at 500 μg/kg. The recoveries spiked in real samples were from 70. 7% to 117.0%. The limits of detection （LODs, l0 times of standard deviation） were in the range of 0. 5 - 500μg/kg. The method has been successfully applied to the simultaneous determination of the 13 N-nitrosamines in rubber products.

关 键 词：固相萃取 超高效液相色谱-电喷雾电离串联质谱 N-亚硝胺 橡胶制品 

分 类 号：O658[理学—分析化学]