食品科学

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正相高效液相色谱法测定腌腊肉制品中磷脂酰胆碱氢过氧化物的含量

任 双,宋 慧,耿志明,王道营,张牧焓,孙 冲,徐为民   

  1. 1.南京农业大学 肉品加工与质量控制教育部重点实验室,江苏 南京 210095;
    2.江苏省农业科学院农产品加工研究所,江苏 南京 210014;
    3.江苏省肉类生产与加工质量安全控制协同创新中心,江苏 南京 210095
  • 出版日期:2016-07-25 发布日期:2016-07-26
  • 通讯作者: 徐为民
  • 基金资助:

    国家自然科学基金青年科学基金项目(31401560);江苏省农业科技自主创新资金项目(CX(13)3081)

Determination of Phosphatidylcholine Hydroperoxide in Dry Cured Meat Products by Normal-Phase High Performance Liquid Chromatography

REN Shuang, SONG Hui, GENG Zhiming, WANG Daoying, ZHANG Muhan, SUN Chong, XU Weimin   

  1. 1. Key Laboratory of Meat Processing and Quality Control, Ministry of Education, Nanjing Agricultural University, Nanjing 210095, China;
    2. Institute of Agricultural Products Processing, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China;
    3. Collaborative Innovation Center of Meat Production and Processing, Nanjing 210095, China
  • Online:2016-07-25 Published:2016-07-26
  • Contact: XU Weimin

摘要:

采用正相高效液相色谱法对腌腊肉制品中的磷脂酰胆碱氢过氧化物(PC-OOH)进行检测。腌腊肉制品中的PC-OOH用氯仿-甲醇(2∶1,V/V)提取,以合成的C16∶0/18∶2 PC-OOH为标样,采用正相高效液相色谱-紫外法进行检测。色谱柱:Lichrosorb Si60(250 mm×4.0 mm,5 μm);流动相:A为水,B为正己烷-异丙醇(3∶2,V/V),采用梯度洗脱;流速:1 mL/min;柱温:30 ℃;检测波长:234 nm。结果表明:C16∶0/18∶2 PC-OOH在20~600 nmol/mL范围内呈现良好的线性关系(R2=0.999 9),检出限为5.8 nmol/mL,定量限为19.4 nmol/mL,不同水平的平均回收率为79.4%~91.9%。实际样品分析显示,农家腊肠A、B和火腿中方样品中PC-OOH的含量比较高,为92.4、106.4 nmol/g和102.5 nmol/g,烟熏肉中未检出PC-OOH。本实验建立的分析方法简便快捷、具有较好的灵敏度和可靠性,可用于腌腊肉制品中PC-OOH的定量分析。

关键词: 腌腊肉制品, 1-棕榈酰-2-亚油酰-磷脂酰胆碱, 氢过氧化物, 正相高效液相色谱法

Abstract:

A normal-phase high-performance liquid chromatographic (HPLC) method was established to determine
phosphatidylcholine monohydroperoxide (PC-OOH) in dry cured meat products. The PC-OOH in dry cured meat samples
was extracted with chloroform/methanol (2:1, V/V), followed by determination by normal-phase HPLC connected to a
photo-diode array detector (HPLC-PAD) with synthetic C16:0/18:2 PC-OOH as the standard. The chromatographic conditions
were established using a Lichrosorb Si60 column (250 mm × 4.0 mm, 5 μm) with a mobile phase consisting of water and
n-hexane/isopropanol (3:2, V/V) in gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at
234 nm. Results indicated that the linearity ranged from 20 to 600 nmol/mL (R2 = 0.999 9), and the limits of detection (LOD)
and limits of quantification (LOQ) were 5.8 nmol/mL and 19.4 nmol/mL, respectively. The recoveries from spiked samples
at concentration levels of 32–240 nmol/g were in the range of 79.4%–91.9%. The contents of PC-OOH in farm-made sausage
A, B and Chinese ham samples were 92.4, 106.4 and 102.5 nmol/g, respectively, while PC-OOH in smoked meat was not
detected. This method proved to be of high maneuverability, excellent sensitivity and high accuracy, and could be used for
quantitative analysis of PC-OOH in dry cured meat samples.

Key words: dry cured meat, 1-palmitoyl-2-linoleoyl-phosphatidylcholine, hydroperoxide, normal-phase HPLC

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