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液相色谱法检测食用油中9种抗氧化剂的优化

Optimization of liquid chromatography for the determination of nine antioxidants in edible oils

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目的 明确和优化油类样品 9 种抗氧化剂的检测方法.方法 油类样品用 3 mL乙腈饱和的正己烷溶液溶解后,用 3 mL含AP的正己烷饱和的乙腈重复提取 5 次,合并 5 次提取液.用C18 固相萃取柱净化,全部提取液和洗脱液一起收集浓缩至0.2 mL,最后用乙腈定容至2 mL.结果 9种抗氧化剂在1.0~60.0 μg/mL范围内线性关系良好,相关系数均大于0.99;回收率91.2%~108.8%之间,相对标准偏差(RSD)为0.6%~10.0%;检出限在0.2~2.0 mg/kg范围,定量限在0.6~6.0 mg/kg范围.结论 本方法通过优化提取次数、净化方法和洗脱体积,9种抗氧化剂的回收率均有显著提高,其中提取次数对BHT、DG的回收率影响较大.
Objective Clarify and optimize the detection methods for 9 antioxidants in oil samples.Methods After dissolving the oil sample in 3 mL of n-hexane solution saturated with acetonitrile,repeat the extraction 5 times with 3 mL of n-hexane saturated acetonitrile containing AP,and merge the 5 extraction solutions.Purify with a C18 solid-phase extraction column,collect and concentrate all extraction and eluent together to 0.2 mL,and finally make up to 2 mL with acetonitrile.Results 9 antioxidants linear relationship is good within the range of 1.0 to 60.0 μg/mL,and the correlation coefficients are all greater than 0.99;the recovery rate ranges from 91.2% to 108.8%,with a relative standard deviation(RSD)of 0.6% to 10.0%;the detection limit is within the range of 0.2~2.0 mg/kg,and the quantitative limit is within the range of 0.6~6.0 mg/kg.Conclusion This method optimizes the extraction frequency,purification method,and elution volume,and significantly improves the recovery rates of 9 antioxidants.The extraction frequency has a significant impact on the recovery rate of BHT and DG.

edible oilantioxidantoptimizationextraction frequencyC18 solid-phase extraction column

陆秀青、韦云莹、农子明、马炜烨

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广西壮族自治区粮油质量检验中心,南宁 530031

食用油 抗氧化剂 优化 提取次数 C18固相萃取柱

2024

实验室检验
中国检验检测学会

实验室检验

ISSN:2097-261X
年,卷(期):2024.2(7)