食品科学 ›› 2021, Vol. 42 ›› Issue (4): 271-277.doi: 10.7506/spkx1002-6630-20190703-039

• 安全检测 • 上一篇    下一篇

正相高效液相色谱法同时测定肉制品中4 种羟基十八碳二烯酸异构体的含量

刘婷,熊强,耿志明,徐为民   

  1. (1.南京工业大学食品与轻工学院,江苏?南京 211816;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:2021-02-25 发布日期:2021-02-25
  • 基金资助:
    国家自然科学基金面上项目(31671877);江苏省自然科学基金项目(BK20171324)

Simultaneous Measurement of Four Hydroxyoctadecadienoic Acid Isomers in Meat Products by Normal-phase High Performance Liquid Chromatography

LIU Ting, XIONG Qiang, GENG Zhiming, XU Weimin   

  1. (1. College of Food Science and Light Industry, Nanjing Tech University, Nanjing 211816, China; 2. Institute of Agricultural Products Processing, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China; 3. Jiangsu Collaborative Innovation Center of Meat Production and Processing, Quality and Safety Control, Nanjing 210095, China)
  • Online:2021-02-25 Published:2021-02-25

摘要: 为建立同时测定肉制品中13-羟基-9Z,11E-十八碳二烯酸(13-hydroxy-9Z,11E-octadecadienoic acid,13-Z,E-HODE)、13-羟基-9E,11E-十八碳二烯酸(13-hydroxy-9E,11E-octadecadienoic acid,13-E,E-HODE)、9-羟基-10Z,12E-十八碳二烯酸(9-hydroxy-10Z,12E-octadecadienoic acid,9-Z,E-HODE)、9-羟基-10E,12E-十八碳二烯酸(9-hydroxy-10E,12E-octadecadienoic acid,9-E,E-HODE)的高效液相色谱检测方法,肉制品中的13-Z,E-HODE、13-E,E-HODE、9-Z,E-HODE和9-E,E-HODE经甲醇提取、采用Sep-Pak C18柱净化浓缩后,在硅胶柱Absolute SiO2(250 mm×4.6 mm,5 μm)上以正己烷-异丙醇-乙酸(98.3∶1.6∶0.1,V/V)为流动相进行分离,选用二极管阵列检测器在234 nm进行测定。结果表明,13-Z,E-HODE、13-E,E-HODE、9-Z,E-HODE和9-E,E-HODE分别在质量浓度为0.5~20.0、0.25~10.0、0.75~12.5 μg/mL和0.5~7.5 μg/mL的范围内线性关系良好(R2分别为0.999 4、0.999 2、0.999 2、0.999 6),检出限分别为0.075、0.035、0.090、0.060 μg/g,定量限分别为0.25、0.12、0.32、0.20 μg/g,不同添加水平的平均回收率分别为89.03%、89.03%、89.33%、87.93%。对18 种肉制品含量分析表明,所有样本都含有13-Z,E-HODE、13-E,E-HODE、9-Z,E-HODE和9-E,E-HODE,含量分别为1.73~9.10、0.56~5.79、2.37~11.02、0.78~5.82 μg/g。综上,建立的检测方法快捷、准确、重复性好,可用于同时测定肉制品中13-Z,E-HODE、13-E,E-HODE、9-Z,E-HODE和9-E,E-HODE的含量。

关键词: 羟基十八碳二烯酸;脂质氧化;亚油酸;高效液相色谱

Abstract: In this study, a high performance liquid chromatography (HPLC) method was established for simultaneous determination of 13-hydroxy-9Z,11E-octadecadienoic acid (13-Z,E-HODE), 13-hydroxy-9E,11E-octadecadienoic acid (13-E,E-HODE), 9-hydroxy-10Z,12E-octadecadienoic acid (9-Z,E-HODE) and 9-hydroxy-10E,12E-octadecadienoic acid (9-E,E-HODE) in meat products. The analytes were extracted from samples with methanol, purified by Sep-Pak C18 column, and then separated using isocratic elution on an Absolute SiO2 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of n-hexane, isopropanol and acetic acid (98.3:1.6:0.1, V/V) before being detected at 234 nm using a photo-diode array (PDA). The results indicated that the method displayed a good linearity within the concentration ranges of 0.5–20.0 μg/mL (R2 = 0.999 4) for 13-Z,E-HODE, and 0.25–10.0 μg/mL (R2 = 0.999 2) for 13-E,E-HODE, 0.75–12.5 μg/mL (R2 = 0.999 2) for 9-Z,E-HODE and 0.5–7.5 μg/mL (R2 = 0.999 6) for 9-E,E-HODE, respectively. The detection limits (LODs) for 13-Z,E-HODE, 13-E,E-HODE, 9-Z,E-HODE and 9-E,E-HODE were 0.075, 0.035, 0.090 and 0.060 μg/g, respectively, and the limits of quantification (LOQs) were 0.25, 0.12, 0.32 and 0.20 μg/g, respectively. The average recoveries from spiked samples were 89.03%, 89.03%, 89.33% and 87.93%, respectively. When this method was used to analyze 18 meat products, all the samples contained 13-Z,E-HODE, 13-E,E-HODE, 9-Z,E-HODE and 9-E,E-HODE at levels of 1.73–9.10, 0.56–5.79, 2.37–11.02 and 0.78–5.82 μg/g, respectively. In conclusion, this method was proved to be fast, accurate and reproducible, and could be used for the simultaneous quantitative analysis of 13-Z,E-HODE, 13-E,E-HODE, 9-Z,E-HODE and 9-E,E-HODE in meat products.

Key words: hydroxyoctadecadienoic acid; lipid oxidation; linoleic acid; high performance liquid chromatography

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