色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 89-94.DOI: 10.3724/SP.J.1123.2013.08003

• 技术与应用 • 上一篇    下一篇

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

陈婷1,3, 温裕云2,3, 欧延2, 弓振斌1,3   

  1. 1. 厦门大学近海海洋环境国家重点实验室, 福建 厦门 361102;
    2. 福建远东技术服务有限公司, 福建 泉州 362006;
    3. 厦门大学环境与生态学院, 福建 厦门 361102
  • 收稿日期:2013-08-01 修回日期:2013-09-02 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 弓振斌
  • 基金资助:

    泉州市科技项目(2012FZ17).

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

CHEN Ting1,3, WEN Yuyun2,3, OU Yan2, GONG Zhenbin1,3   

  1. 1. State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361102, China;
    2. Fujian PFI Fareast Testing & Technology Services Co., Ltd., Quanzhou 362006, China;
    3. College of the Environment & Ecology, Xiamen University, Xiamen 361102, China
  • Received:2013-08-01 Revised:2013-09-02 Online:2014-01-08 Published:2013-12-26

PDF

374

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500 μg/kg、其他组分均为50 μg/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0.5~500 μg/kg。方法可应用于橡胶制品中13种N-亚硝胺的测定。

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

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 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 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 500 μg/kg. The recoveries spiked in real samples were from 70.7% to 117.0%. The limits of detection (LODs, 10 times of standard deviation) were in the range of 0.5-500 μg/kg. The method has been successfully applied to the simultaneous determination of the 13 N-nitrosamines in rubber products.

Key words: N-nitrosamines, rubber products, solid phase extraction (SPE), ultra high performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS)

中图分类号: