气相色谱法测定水产品中蜡酯

Determination of wax esters in seafoods by gas chromatography

中文关键词:  水产品  蜡酯  气相色谱法  固相萃取

英文关键词:seafood  wax ester  gas chromatography  solid-phase extraction

中文摘要:

      目的 建立一种气相色谱法检测水产品中蜡酯组成和含量的分析方法。方法 采用氯仿-甲醇提取, 硅胶固相萃取柱净化, 正己烷-乙醚洗脱, 得到待测样本。采用气相色谱和气相色谱-质谱法分析几种含有蜡酯的典型水产品中蜡酯的具体组成, 选取了C30、C32、C34、C36、C38蜡酯作为检测目标物, 使用气相色谱进行检测, 内标法定量。结果 对于含有蜡酯的典型水产品, 以肉豆蔻酸月桂醇酯(C26酯)为内标物进行定量。该方法的峰形良好, 检出限为0.6 μg/mL, 定量限为2.0 μg/mL, 线性方程r2为0.9995~0.9999, 精密度实验得到的相对标准偏差均小于5%, 阳性样本中加标回收率为95.29%~103.91%, 阴性样本中加标回收率为86.52%~105.98%。结论 本方法可以实现水产品蜡酯成分的有效检测, 为市场监管、风险评估等工作提供技术支持。

英文摘要:

      Objective To establish an analytical method for detecting the composition and content of wax esters in seafoods by gas chromatography. Methods The samples were extracted with chloroform-methanol, purified by silica gel solid-phase extraction column, and eluted with n-hexane-ether to obtain the samples to be tested. The specific compositions of wax esters in several typical seafoods containing wax esters were analyzed by gas chromatography and gas chromatography-mass spectrometry. C30, C32, C34, C36 and C38 wax esters were selected as the detection targets, which were detected by gas chromatography with internal standard method for quantification. Results For typical seafoods containing wax esters, lauryl myristate (C26 ester) was used as the internal standard for quantification. The peak shapes of this method were good, the limits of detection were 0.6 μg/mL, the limits of quantification were 2.0 μg/mL, and the r2 of linear equation were between 0.9995?0.9999. The relative standard deviations of precision experiments were all less than 5%, the recoveries of spiked samples in positive samples were 95.29%?103.91% and those in negative samples were 86.52%?105.98%. Conclusion This method can realize the effective detection of wax esters in seafoods, and provide technical support for market supervision and risk assessment.