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

doi:10.3724/SP.J.1123.2013.08003

Abstract

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)

CLC Number:

O658

CHEN Ting, WEN Yuyun, OU Yan, GONG Zhenbin. Determination of N-nitrosamines in rubber products by solid phase extraction purification and ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2014, 32(1): 89-94.

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