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中国精品科技期刊2020
姜春姣, 江芸, 耿志明, 宋慧, 张牧焓, 王道营, 徐为民. 正相高效液相色谱法同时测定腌腊肉制品中13-HODE和9-HODE含量[J]. 食品工业科技, 2017, (24): 268-273. DOI: 10.13386/j.issn1002-0306.2017.24.052
引用本文: 姜春姣, 江芸, 耿志明, 宋慧, 张牧焓, 王道营, 徐为民. 正相高效液相色谱法同时测定腌腊肉制品中13-HODE和9-HODE含量[J]. 食品工业科技, 2017, (24): 268-273. DOI: 10.13386/j.issn1002-0306.2017.24.052
JIANG Chun-jiao, JIANG Yu, GENG Zhi-ming, SONG Hui, ZHANG Mu-han, WANG Dao-ying, XU Wei-min. Simultaneous determination of 13-HODE and 9-HODE in cured meat products by normal-phase HPLC[J]. Science and Technology of Food Industry, 2017, (24): 268-273. DOI: 10.13386/j.issn1002-0306.2017.24.052
Citation: JIANG Chun-jiao, JIANG Yu, GENG Zhi-ming, SONG Hui, ZHANG Mu-han, WANG Dao-ying, XU Wei-min. Simultaneous determination of 13-HODE and 9-HODE in cured meat products by normal-phase HPLC[J]. Science and Technology of Food Industry, 2017, (24): 268-273. DOI: 10.13386/j.issn1002-0306.2017.24.052

正相高效液相色谱法同时测定腌腊肉制品中13-HODE和9-HODE含量

Simultaneous determination of 13-HODE and 9-HODE in cured meat products by normal-phase HPLC

  • 摘要: 采用高效液相色谱对腌腊肉制品中的13-羟基十八碳二烯酸(13-HODE)和9-羟基十八碳二烯酸(9-HODE)进行检测。腌腊肉制品中的13-HODE和9-HODE用甲醇提取,经C18固相萃取柱净化,以正己烷/异丙醇/乙酸(98∶2∶0.5,v/v/v)为流动相,在Lichrosorb Si 60(250×4.0 mm,5μm)色谱柱上分离,选用二极管阵列检测器在234 nm进行检测。结果表明:13-HODE和9-HODE分别在0.520和1.012.5μg/m L范围内线性良好(R2分别为0.9994和0.9990),检测限分别为0.075、0.15μg/g,定量限分别为0.25、0.5μg/g。不同添加水平的平均回收率分别为88.2%和86.0%。对14种腌腊肉制品的分析结果显示,所有样本均含有13-HODE和9-HODE,范围分别为:1.2167.54和0.63139.20μg/g。本实验建立的检测方法操作简单、易于普及,具有良好的灵敏度和准确性,可以满足腌腊肉制品中13-HODE和9-HODE含量的同时分析。 

     

    Abstract: 13-hydroxy-9, 11-octadecadienoic acid ( 13-HODE) and 9-hydroxy-9, 11-octadecadienoic acid ( 9-HODE) in cured meat products were detected with high performance liquid chromatography connected to a diode array detector ( HPLCDAD) . The analytes, extracted with methanol and cleaned up by solid phase cleanup with C18 column, were separated on a Lichrosorb Si 60 column ( 250 × 4.0 mm, 5 μm) with a mobile phase consisting of n-hexane/isopropanol/acetic acid ( 98∶ 2∶ 0.5, v/v/v) in isocratic elution and the detection wavelength was set at 234 nm.The results indicated that 13-HODE and 9-HODE displayed good linearity in the ranges of 0.5 ~ 20.0 μg/m L ( R2= 0.9994) and 1 ~ 12.5 μg/m L ( R2= 0.9990) , respectively.Limits of detection for 13-HODE and 9-HODE were 0.075 and 0.15 μg/g, respectively, and quantification limits were 0.25 and 0.5 μg/g, respectively.The average recoveries spiked at different levels were 88.2% and 86.0%, respectively.The method was successfully employed to detect the analytes in 14 cured meat products and the results showed that all samples contained 13-HODE and 9-HODE ranging from 1.2167.54 μg/g and 0.63139.20 μg/g, respectively.This method proved to be of high maneuverability as well as excellent sensitivity and accuracy, and could be used for quantitative analysis of13-HODE and 9-HODE in cured meat samples simultaneously.

     

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