【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30 min,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。更多还原

【Abstract】 A method using C18 solid phase extraction(SPE)for purification and ultra high performance liquid chromatography(UHPLC)coupled with electrospray ionization tandem mass spectrometry(ESI-MS/MS)for detection was developed to simultaneously determine 13 Nnitrosamines in rubber products.The analytes were extracted with methanol(60℃,30 min)with the aid of ultrasonic technique and then purified by a C18 SPE cartridge.The analytes were separated on a C18 chromatographic column and qualitatively and quantitatively detected by a mass spectrometer with positive ESI at multiple reaction monitoring(MRM)mode.The operating 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 50 μg/kg for all analytes except N-nitrosodimethylamine(NDMA)and N-nitrosodiethylamine(NDEA)which were spiked at 500μg/kg.The recoveries spiked in real samples were from70.7% to 117.0%.The limits of detection(LODs,10 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.更多还原