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Determination of Eleven N-Nitrosamines in Animal Derived Foods by Gas Chromatography-Tandem Mass Spectrometry after Pass-Through Solid Phase Extraction |
WANG Yanli, LIANG Xiuqing, CHEN Qianqian, LI Fangfang, LI Jie, CHEN Keyun, TIAN Qiyan, LI Xia, LIU Yanming |
Shandong Research Center of Engineering and Technology for Saefty Inspection of Food and Drug, Key Laboratory of SupervisingT echnology for Meat and Meat Products for State Market Regulation, Shandong Institute for Food and Drug Control, Ji’nan 250101, China |
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Abstract A method was developed for the determination of 11 N-nitrosamines in animal derived foods by pass-through solid phase extraction coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The rehydrated samples were extracted with acetonitrile and rapidly purified by using a Prime HLB solid phase extraction column (200 mg/6 mL). The target compounds were detected in the multiple reaction monitoring (MRM) mode, and quantified by the matrix matched external standard method. The calibration curves for the 11 N-nitrosamines were linear in the concentration range of 0.5–500.0 ng/mL, with correlation coefficients of 0.999 4–0.999 8. The limits of detection (LODs) and the limits of quantitation (LOQs) were 0.2–0.3 and 0.5–1.0 μg/kg, respectively. The average recoveries at spiked levels of 1, 4 and 10 μg/kg ranged from 80.1% to 97.4%, and the relative standard deviations (RSDs) were between 2.3% and 8.8%. The extraction and purification time required by this method was only 15 min/sample and greatly shortened compared with GB 5009.26-2016, and the detection efficiency was increased by 10 times. This method allows rapid detection of N-nitrosamines residues in animal derived foods.
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