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液相色谱法检测食用油中9种抗氧化剂的优化 被引量:3

Optimization of liquid chromatography for the determination of nine antioxidants in edible oils
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摘要 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1.0~60.0μg/m L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 60.0μg/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.
作者 陆秀青 韦云莹 农子明 马炜烨 LU Xiu-Qing;WEI Yun-Ying;NONG Zi-Ming;MA Wei-Ye(Guangxi Zhuang Autonomous Region Grain and Oil Quality Inspection Center,Nanning 530031,China)
出处 《实验室检测》 2024年第7期45-48,共4页 Laboratory Testing
关键词 食用油 抗氧化剂 优化 提取次数 C18固相萃取柱 edible oil antioxidant optimization extraction frequency C18 solid-phase extraction column
作者简介 通信作者:农子明,工程师,研究方向为粮油质量分析。E-mail:347998976@qq.com;陆秀青,工程师,研究方向为粮油质量分析。
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