气相色谱-质谱法测定大菱鲆肌肉中羧甲基赖氨酸含量

建立了大菱鲆肌肉中羧甲基赖氨酸（CML）的气相色谱-质谱（GC-MS）检测方法。以大菱鲆为研究对象,选用三氯甲烷/丙酮对样品进行脱脂,经硼氢化钠还原、蛋白水解、净化、衍生化（酯化与酰化）后,进行GC-MS选择离子监测（SIM）模式检测。选取m/z 392为定量离子,m/z 392,365,333,305为定性离子。结果表明,CML三氟乙酰甲酯化衍生物峰面积与浓度在1~200μg/L范围内呈良好线性关系,方法检出限为1 mg/kg,定量限为5 mg/kg,3个加标水平（10,150和350 mg/kg）下的平均回收率在100%~104%之间,相对标准偏差RSD〈5%（n=5）。...

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Bibliographic Details
Published in分析化学 Vol. 43; no. 8; pp. 1187 - 1192
Main Author 王菁 田盛兰 孙伟红 林洪 李振兴
Format Journal Article
LanguageChinese
Published 中国海洋大学食品科学与工程学院,青岛,266003%中国水产科学研究院黄海水产研究所,青岛,266071 2015
Subjects
大菱鲆
气相色谱-质谱
羧甲基赖氨酸
衍生化
Nε-carboxymethyl-lysine
大菱鲆
气相色谱-质谱
衍生化
羧甲基赖氨酸
Turbot
Gas chromatography-mass spectrometry
Derivatization
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Summary:建立了大菱鲆肌肉中羧甲基赖氨酸（CML）的气相色谱-质谱（GC-MS）检测方法。以大菱鲆为研究对象,选用三氯甲烷/丙酮对样品进行脱脂,经硼氢化钠还原、蛋白水解、净化、衍生化（酯化与酰化）后,进行GC-MS选择离子监测（SIM）模式检测。选取m/z 392为定量离子,m/z 392,365,333,305为定性离子。结果表明,CML三氟乙酰甲酯化衍生物峰面积与浓度在1~200μg/L范围内呈良好线性关系,方法检出限为1 mg/kg,定量限为5 mg/kg,3个加标水平（10,150和350 mg/kg）下的平均回收率在100%~104%之间,相对标准偏差RSD〈5%（n=5）。
Bibliography:WANG Jing, TIAN Sheng-Lan, SUN Wei-Hong, LIN I-Iong , LI Zhen-Xing 1（ Food Science and Technology College, Ocean University of China, Qingdao 266003, China） z（ Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China）
Nε-carboxymethyl-lysine ; Turbot; Gas chromatography-mass spectrometry ; Derivatization
22-1125/O6
A method was developed to determine the content of Nε-carboxymethyl-lysine （CML） in the muscle tissues of turbot by gas chromatography-mass spectrometric method. Turbot was selected as the research object, homogenized muscle tissue samples of turbot defatted by chloroform/acetone were pretreated followed by reduction, acid hydrolysis, purifying and derivatization （esterification and acylation）. The ion of m/z 392 was selected as quantitative ion and the ions of m/z 392, 365, 333, 305 were selected as qualitative ions in selected ion monitoring mode. The range of the linear calibration curve of CML derivative peak area and concentration extended from 1 μg/L to
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.150203