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SPE-LC-MS/MS法检测肉制品中羧甲基赖氨酸与羧乙基赖氨酸

发表时间:2014-10-15  浏览量:1617  下载量:641
全部作者: 高畅,何志勇,曾茂茂,陈洁
作者单位: 爱博才思分析仪器贸易有限公司;江南大学食品科学与技术国家重点实验室
摘 要: 建立了一种基于固相萃取(solid-phase extraction, SPE)-液相色谱(liquid chromatography, LC)-三重四级杆质谱(triple quadrupole mass spectrometry, MS/MS)(SPE-LC-MS/MS)检测肉制品中2种晚期糖基化末端终产物(advanced glycation end products,AGEs)羧甲基赖氨酸[Nε-(carboxymethyl)lysine, CML]和羧乙基赖氨酸[Nε-(carboxyethyl)lysine, CEL]的方法。样品用正己烷除去脂肪,硼氢化钠还原,酸水解蛋白质,Oasis MCX小柱净化。以乙腈-5 mmol/L九氟戊酸作为流动相,采用X-Bridge C18色谱柱,选择电喷雾源(electron spray ionization,ESI)正离子模式(ESI+)和多重反应监测(multiple reaction monitoring, MRM)进行LC-MS/MS分析,同位素内标稀释法定量。该方法检出限为0.13~0.28 μg/g,加标回收率为88.57%~103.15%,相对标准偏差(relative standard deviation, RSD)为4.34%~13.72%. 最后对市场上若干种肉制品进行检测,各样品中均有检出,其中肉松中CML含量最高,达到81.71 μg/g,猪肉脯中CEL含量最高,可达112.43 μg/g.
关 键 词: 食品检验学;晚期糖基化终产物;固相萃取;液相色谱-质谱;肉制品
Title: Determination of Nε-(carboxymethyl)lysine and Nε-(carboxyethyl) lysine in meat product by SPE-LC-MS/MS
Author: GAO Chang1, HE Zhiyong2, ZENG Maomao2, CHEN Jie
Organization: AB Sciex Analytical Instrument Trading Co. Ltd.; State Key Laboratory of Food Science & Technology, Jiangnan University
Abstract: In this paper, a reliable method based on solid-phase extraction-liquid chromatography-triple quadrupole mass spectrometry (SPE-LC-MS/MS) was developed to determine two typical advanced glycation end products(AGEs), namely Nε-(carboxymethyl)lysine (CML) and Nε-(carboxyethyl)lysine (CEL) in meat products. Sample was reduced by sodium borohydride after removing lipid. After hydrolysis, sample was cleaned up by Oasis MCX SPE cartridge. Then the sample was separated by X-Bridge C18 column with acetonitrile and 5 mmol/L nonafluoropentanoic acid aqueous solution as mobile phases. LC-MS/MS analysis was conduct using electron spray ionization (ESI) in the positive ion mode (ESI+) and multiple reaction monitoring (MRM) mode, and was quantified by stable isotope dilution method. The limit of detection ranged from 0.13 μg/g to 0.28 μg/g. The average recovery of CML and CEL of meat products at three spiked levels ranged from 88.57% to 103.15% with relative standard deviation (RSD) in the range of 4.34% to 13.72%. Several kinds of commercial meat products were detected, and both CML and CEL were found in all of the meat products. The highest contents of CML and CEL were detected in dried meat floss (81.71 μg/g) and dried pork slice (112.43 μg/g), respectively.
Key words: food inspection; advanced glycation end products; solid-phase extraction; liquid chromatography-triple quadrupole mass spectrometry; meat product
发表期数: 2014年10月第19期
引用格式: 高畅,何志勇,曾茂茂,等. SPE-LC-MS/MS法检测肉制品中羧甲基赖氨酸与羧乙基赖氨酸[J]. 中国科技论文在线精品论文,2014,7(19):1986-1991.
 
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