Establishment of a QuEChERS-FaPEx Rapid Analytical Method for N-Nitrosamines in Meat Products

建立QuEChERS-FaPEx快速分析方法测定肉制品中的N-亚硝胺

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Abstract

This study aimed to establish a fast and efficient method for the determination of N-nitrosamines (NAs) in meat products by integrating two sample preparation techniques-QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and FaPEx (Fast Pesticide Extraction)-with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chromatographic separation was performed on a Poroshell 120 Phenyl Hexyl column using a gradient elution of acetonitrile and 0.01% formic acid at a flow rate of 0.3 mL/min and a column temperature of 25 °C. Under these conditions, nine NAs and one internal standard were completely separated within 11 min with selective reaction monitoring mode (SRM) for detection. Samples were first extracted with QuEChERS powder using acetonitrile containing 0.1% formic acid, followed by purification with a FaPEx-Chl cartridge. This combined approach demonstrated superior performance compared with traditional solvent extraction or QuEChERS extraction alone. The recoveries of the developed method ranged from 76% to 111% and 52% to 103% at spiking levels of 50 ng/g and 20 ng/g, respectively. The limits of detection (LOD) and quantification (LOQ) were 0.002-0.3 ng/g and 0.006-1.00 ng/g, respectively. The inter-day and intra-day precisions (RSD%) ranged from 2.7% to 17% and 2.9% to 17%, respectively. These results indicate that the proposed method is among the most time-efficient and effective analytical approaches currently available for the determination of NAs in meat products.

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