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

作　　者：姜春姣 江芸[1] 耿志明[2] 宋慧[2] 张牧焓[2] 王道营[2] 徐为民[2,3] 

机构地区：[1]南京师范大学金陵女子学院食品科学系,江苏南京210097 [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　　处：《食品工业科技》2017年第24期268-273,277,共7页Science and Technology of Food Industry

基　　金：国家自然科学基金资助项目(31671877)

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0.5~20和1.0~12.5μg/m L范围内线性良好(R^2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:1.2~167.54和0.63~139.20μg/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。13-hydroxy-9,11 - octadecadienoic acid （ 13 - HODE ） and 9 - hydroxy- 9,11 - oetadecadienoic acid （ 9 - HODE ） in cured meat products were detected with high performance liquid chromatography connected to a diode array detector（ HPLC- DAD） .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/mL（ R2 = 0.9994）and 1-12.5μg/mL （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 0.5μg/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 1.2-167.54 μg/g and 0.63-139.20 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 of 13-HODE and 9-HODE in cured meat samples simultaneously.

关 键 词：亚油酸 腌腊肉制品 13-HODE 9-HODE 高效液相色谱法 

分 类 号：TS201.6[轻工技术与工程—食品科学]