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采用QuEChERS样品前处理结合反吹式气相色谱-串联质谱法分析熟培根中的亚硝胺

Analysis of Nitrosamines in Cooked Bacon by QuEChERS Sample Preparation and Gas Chromatography-Tandem Mass Spectrometry with Backflushing.

作者信息

Lehotay Steven J, Sapozhnikova Yelena, Han Lijun, Johnston John J

机构信息

Eastern Regional Research Center, Agricultural Research Service, U.S. Department of Agriculture , 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, United States.

College of Science, China Agricultural University , 2 Yuanmingyuan West Road, Beijing 100193, People's Republic of China.

出版信息

J Agric Food Chem. 2015 Dec 2;63(47):10341-51. doi: 10.1021/acs.jafc.5b04527. Epub 2015 Nov 17.

Abstract

Nitrites are added as a preservative to a variety of cured meats, including bacon, to kill bacteria, extend shelf life, and improve quality. During cooking, nitrites in the meat can be converted to carcinogenic nitrosamines (NAs), the formation of which is mitigated by the addition of antioxidants. In the past, the U.S. Department of Agriculture (USDA) Food Safety and Inspection Service (FSIS) monitored NAs in pan-fried bacon, but FSIS terminated monitoring of NAs in the 1990s due to the very low levels found. FSIS recently chose to conduct a risk assessment of NAs in cooked bacon to determine if current levels warrant routine monitoring of NAs again. To meet FSIS needs, we developed, validated, and implemented a new method of sample preparation and analysis to test cooked bacon for five NAs of most concern, which consist of N-nitroso-dimethylamine, -diethylamine, -dibutylamine, -piperidine, and -pyrrolidine. Sample preparation was based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach and analysis by gas chromatography-tandem mass spectrometry. Ruggedness was improved markedly in the analysis of the complex fatty extracts by backflushing the guard column, injection liner, and half of the analytical column after every injection. Validation results were acceptable with recoveries of 70-120% and <20% RSDs for the five NAs, with a reporting limit of 0.1 ng/g. NA concentrations in 48 samples were all <15 ng/g, with most <1 ng/g and many <0.1 ng/g. Also, microwave cooking of bacon gave slightly lower concentrations overall compared to pan-frying.

摘要

亚硝酸盐被添加到包括培根在内的各种腌制肉类中作为防腐剂,以杀灭细菌、延长保质期并提高品质。在烹饪过程中,肉类中的亚硝酸盐可转化为致癌的亚硝胺(NAs),添加抗氧化剂可减少亚硝胺的形成。过去,美国农业部(USDA)食品安全与检验局(FSIS)监测煎培根中的亚硝胺,但由于检测到的含量极低,FSIS在20世纪90年代终止了对亚硝胺的监测。FSIS最近选择对熟培根中的亚硝胺进行风险评估,以确定当前含量是否再次需要对亚硝胺进行常规监测。为满足FSIS的需求,我们开发、验证并实施了一种新的样品制备和分析方法,以检测熟培根中最受关注的五种亚硝胺,它们分别是N-亚硝基二甲胺、-二乙胺、-二丁胺、-哌啶和-吡咯烷。样品制备基于QuEChERS(快速、简便、廉价、有效、耐用且安全)方法,并通过气相色谱-串联质谱法进行分析。通过每次进样后反吹保护柱、进样口衬管和一半分析柱,在分析复杂脂肪提取物时显著提高了耐用性。验证结果可接受,五种亚硝胺的回收率为70-120%,相对标准偏差<20%,报告限为0.1 ng/g。48个样品中的亚硝胺浓度均<15 ng/g,大多数<1 ng/g,许多<0.1 ng/g。此外,与煎制相比,用微波炉烹饪培根总体上亚硝胺浓度略低。

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