食品科学

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糖醋排骨中羧甲基赖氨酸分析方法的建立及其烹饪过程中动态变化

贾寒冰,申明月,谢俊华,刘玲玲,聂少平   

  1. 南昌大学 食品科学与技术国家重点实验室,江西 南昌 330047
  • 出版日期:2015-12-25 发布日期:2015-12-24
  • 通讯作者: 聂少平
  • 基金资助:

    “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)

Establishment of Analytical Method for Nε-(carboxymethyl)lysine in Sweet and Sour Pork Ribs and Its Dynamic Change during the Cooking Process

JIA Hanbing, SHEN Mingyue, XIE Junhua, LIU Lingling, NIE Shaoping   

  1. State Key Laboratory of Food Science and Technology, Nangchang University, Nangchang 330047, China
  • Online:2015-12-25 Published:2015-12-24
  • Contact: NIE Shaoping

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。

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

Abstract:

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 ribs. Samples were reduced by sodium borohydride after removing
lipid. HCl 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.

Key words: advanced glycation end products, Nε-(carboxymethyl)lysine, sweet and sour pork ribs, high performance liquid chromatography triple quadrupole mass spectrometry, multiple reaction monitoring

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