气相色谱-三重四级杆质谱法测定多不饱和脂肪酸  

Determination of polyunsaturated fatty acids by gas chromatography-triple quadrupole mass spectrometry

作　　者：牛立沙 孟志娟 赵丽敏 黄云霞 李强[1] 张亚丽 NIU Lisha;MENG Zhijuan;ZHAO Limin;HUANG Yunxia;LI Qiang;ZHANG Yali(Hebei Food Safety Key Laboratory/Key Laboratory of Special Food Supervision Technology for State Market Regulation/Hebei Engineering Research Center for Special Food Safety and Health/Hebei Food Inspection and Research Institute,Shijiazhuang Hebei,050091,China)

机构地区：[1]河北省食品安全重点实验室/国家市场监管重点实验室(特殊食品监管技术)/特殊食品安全与健康河北省工程研究中心/河北省食品检验研究院,河北石家庄050091

出　　处：《质量安全与检验检测》2023年第1期21-27,共7页QUALITY SAFETY INSPECTION AND TESTING

基　　金：河北省市场监督管理局科研计划项目(2021ZC08);河北省高层次人才资助项目(C20221009)。

摘　　要：多不饱和脂肪酸(PUFAS)是脂肪的主要活性物质。本研究基于气相色谱-三重四级杆质谱(MRM)技术,建立了同时测定7种PUFAS的定性、定量分析方法。结果显示,7种PUFAS的检出限(S/N>3)为3.81~4.52 mg/kg,定量限(S/N>10)为11.4~13.5 mg/kg,在0.020~1.000 mg/mL范围内线性关系良好,线性相关系数R2>0.999。7种PUFAS的添加水平为5、20、50 mg/100 g时,回收率分别为102.6%~107.1%、97.4%~100.3%、98.5%~100.4%,相对标准偏差(RSD)分别为0.953%~2.31%、0.809%~2.39%、0.310%~4.22%。应用该法对市场抽检的样品进行测定,结果发现,样品中含有的主要PUFAS为亚油酸(LA)、α-亚麻酸(ALA)、二十碳四烯酸(ARA)、二十二碳六烯酸(DHA)。该方法的前处理经优化后,大大缩短了检测时间,减少了试剂的使用量,降低了经济成本。与气相色谱法相比,MRM法更加精确、灵敏、可靠,适用于PUFAS的定性、定量分析。Polyunsaturated fatty acids(PUFAS)are the main active substances of fat.This study established a qualitative and quantitative analysis method for the simultaneous determination of 7 kinds of PUFAS based on gas chromatography-triple quadrupole mass spectrometry(MRM)technology.The experimental results showed that the detection limit(S/N>3)of 7 kinds PUFAS was 3.81-4.52 mg/kg,and the quantitative limit(S/N>10)was 11.4-13.5 mg/kg.The linear relationship is good in the range of 0.020-1.000 mg/mL,and the linear correlation coefficient R2>0.999.The addition levels of 7 kinds of PUFAS are 5 mg/100 g,20 mg/100 g and 50 mg/100 g,the recoveries were 102.6%-107.1%,97.4%-100.3%,98.5%-100.4%,and the relative standard deviation(RSD)were 0.953%-2.31%,0.809%-2.39%,0.310%-4.22%,respectively.The method is applied to determine the samples sampled from the market.The results showed that the main PUFAS contained in the samples were LA,ALA,ARA and DHA.The pretreatment of this method is optimize,it greatly shortened the experimental time.It reduced the use of reagents and the economic cost.Compared with gas chromatography,MRM method is more accurate,sensitive and reliable.It is applicable to the qualitative and quantitative analysis of PUFAS.

关 键 词：气相色谱-三重四极杆质谱法 多不饱和脂肪酸 实际样品 

分 类 号：D550.10[政治法律—政治学]