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采用微波辅助萃取结合分散微固相萃取和气相色谱-化学电离质谱法测定肉制品中的挥发性 N-亚硝胺。

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.

机构信息

Department of Chemistry, National Central University, Chung-Li 320, Taiwan.

出版信息

Food Chem. 2013 May 1;138(1):227-33. doi: 10.1016/j.foodchem.2012.09.119. Epub 2012 Nov 8.

Abstract

A sensitive procedure, microwave-assisted extraction (MAE) coupled dispersive micro solid-phase extraction (D-μ-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-μ-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-μ-SPE conditions were immersing 100mg of Carboxen™ 1000 adsorbent in the MAE extract. After vigorously shaking for 30 min, the NAms were then desorbed by treatment with 200 μL of dichloromethane. A 10 μL 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.

摘要

一种灵敏的程序,微波辅助萃取(MAE)与分散固相微萃取(D-μ-SPE)相结合,被开发用于从肉类产品中提取 N-亚硝基二甲胺(NDMA)和其他六种挥发性 N-亚硝胺(NAms)。系统研究了影响 MAE 和 D-μ-SPE 效率的参数。对于 MAE,将 5 克均质肉样用 30 毫升 0.025 M 氢氧化钠溶液在 100°C 下提取 10 分钟。D-μ-SPE 的最佳条件是将 100mg Carboxen™1000 吸附剂浸入 MAE 提取物中。剧烈摇晃 30 分钟后,用 200 μL 二氯甲烷处理以解吸 NAms。采用气相色谱-化学电离质谱(GC-CI-MS),采用选择离子储存(SIS)模式,用 10 μL 等分试样进行测定。定量限(LOQs)为 0.03-0.36ng/g。初步结果表明,NDMA 的浓度最高,范围为 0.8 至 3.2ng/g。

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