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Analytical Methods
Determination of volatile N-nitrosamines in meat products by microwave-assisted extraction coupled with dispersive micro solid-phase extraction and gas chromatography – Chemical ionisation mass spectrometry
Man-Chun Huang, Hsin-Chang Chen, Ssu-Chieh Fu, Wang-Hsien Ding ⇑
Department of Chemistry, National Central University, Chung-Li 320, Taiwan
a r t i c l e
i n f o
Article history:
Received 21 May 2012
Received in revised form 12 September
2012
Accepted 23 September 2012
Available online 8 November 2012
Keywords:
Microwave-assisted extraction
Dispersive micro solid-phase extraction
N-nitrosamines
GC–MS
Food analysis
a b s t r a c t
A sensitive procedure, microwave-assisted extraction (MAE) coupled dispersive micro solid-phase extraction (D-l-SPE), was developed to extract N-nitrosodimethylamine (NDMA) and other six volatile
N-nitrosamines (NAms) from meat products. Parameters affecting the efficiency of MAE and D-l-SPE were systematically investigated. For MAE, 5-g of a homogenised meat sample was extracted with
30 mL of a sodium hydroxide (0.025 M) solution at 100 °C for 10 min. The optimum D-l-SPE conditions were immersing 100 mg of Carboxen™ 1000 adsorbent in the MAE extract. After vigorously shaking for
30 min, the NAms were then desorbed by treatment with 200 lL of dichloromethane. A 10 lL aliquot was determined by gas chromatography with chemical ionisation mass spectrometry (GC–CI-MS) using the selected-ion-storage (SIS) mode. The limits of quantitation (LOQs) were 0.03–0.36 ng/g. Preliminary results revealed that NDMA was present in the highest concentration, ranging from 0.8 to 3.2 ng/g.
Ó 2012 Elsevier Ltd. All rights reserved.
1. Introduction
The presence of N-nitrosamines (NAms) in foodstuffs has become a significant public health
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