摘要
采用高效液相色谱-三重四极杆质谱联用技术建立了一种操作简单、稳定性好的检测中式菜肴糖醋排骨中羧甲基赖氨酸（Nε-（carboxymethyl）lysine,CML）的方法.样品用正己烷去脂肪,硼氢化钠还原,盐酸水解蛋白,Oasis MCX固相萃取小柱净化.以5 mmol/L的乙酸铵溶液和甲醇-水（80∶20,V/V）溶液作为流动相,采用Phenomenex Synergi 4 μ Hydro-RP 80A色谱柱,在正离子模式下采用多重反应监测分析,同位素内标法定量.该方法检出限为1.40 μg/g,加标回收率为90.94％～105.26％,相对标准偏差为5.80％～15.46％.采用该分析方法对中式菜肴糖醋排骨加工过程中CML的含量变化进行分析,结果表明,加工温度和加热时间以及糖和油脂的添加均可以显著影响糖醋排骨中CML的含量.
In this study, high performance liquid chromatography-triple quadrupole mass spectrometry （HPLC-MS/ MS） was used to establish a simple and stable method for the detection of advanced glycation end products （AGEs） of Nε（carboxymethyl）lysine （CML） in sweet and sour pork fibs. Samples were reduced by sodium borohydfide after removing lipid. HC1 was then added to hydrolyze the protein in the samples. After hydrolysis, the target compounds were cleaned up by Oasis MCX SPE cartridges and then separated by Phenomenex Synergi 4 μ Hydro-RP 80A column with ammonium acetate aqueous solution and methanol solution as mobile phases. HPLC-MS analysis was conducted using electron spray ionization （ESI） in the positive ion mode （ESI＋） and quantification was performed in multiple-reaction monitoring （MRM） mode by stable isotope dilution method. The limit of detection was 1.40 μg/g and the average recoveries of CML ranged from 90.94% to 105.26% with relative standard deviation （RSD） in the range of 5.80%-15.46%. The contents of CML in Huaiyang style sweet and sour spareribs were analyzed. The results showed that heating time, heating temperature and the addition of sugar and oil caused a significant increase in CML content.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2015年第24期142-146,共5页
Food Science
基金
"十二五"国家科技支撑计划项目(2014BAD04B03)
国家重点基础研究发展计划(973计划)项目(2012CB720805)
教育部"新世纪优秀人才支持计划"项目(NCET-12-0749)
关键词
晚期糖基化末端产物
羧甲基赖氨酸
糖醋排骨
高效液相色谱-三重四极杆质谱联用技术
多重反应监测
advanced glycation end products
Nε（carboxymethyl）lysine
sweet and sour pork ribs
high performance liquid chromatography triple quadrupole mass spectrometry
multiple reaction monitoring
