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中国精品科技期刊2020
刘诗瑶, 吴文林, 肖全伟, 梁恒兴, 苟兴华. 超高效液相色谱-四极杆/静电场轨道阱质谱快速筛查和定量检测食用油脂中的天然辣椒素、合成辣椒素和二氢辣椒素[J]. 食品工业科技, 2020, 41(13): 259-263. DOI: 10.13386/j.issn1002-0306.2020.13.041
引用本文: 刘诗瑶, 吴文林, 肖全伟, 梁恒兴, 苟兴华. 超高效液相色谱-四极杆/静电场轨道阱质谱快速筛查和定量检测食用油脂中的天然辣椒素、合成辣椒素和二氢辣椒素[J]. 食品工业科技, 2020, 41(13): 259-263. DOI: 10.13386/j.issn1002-0306.2020.13.041
LIU Shi-yao, WU Wen-lin, XIAO Quan-wei, LIANG Heng-xing, GOU Xing-hua. Rapid Screeninga nd Quantification of Capsaicin, Dihydrocapsaicin, Nonivamide in Edible Oil by Ultra-high Performance Liquid Chromatography-quadrupole/orbitrap Mass Spectroscopy[J]. Science and Technology of Food Industry, 2020, 41(13): 259-263. DOI: 10.13386/j.issn1002-0306.2020.13.041
Citation: LIU Shi-yao, WU Wen-lin, XIAO Quan-wei, LIANG Heng-xing, GOU Xing-hua. Rapid Screeninga nd Quantification of Capsaicin, Dihydrocapsaicin, Nonivamide in Edible Oil by Ultra-high Performance Liquid Chromatography-quadrupole/orbitrap Mass Spectroscopy[J]. Science and Technology of Food Industry, 2020, 41(13): 259-263. DOI: 10.13386/j.issn1002-0306.2020.13.041

超高效液相色谱-四极杆/静电场轨道阱质谱快速筛查和定量检测食用油脂中的天然辣椒素、合成辣椒素和二氢辣椒素

Rapid Screeninga nd Quantification of Capsaicin, Dihydrocapsaicin, Nonivamide in Edible Oil by Ultra-high Performance Liquid Chromatography-quadrupole/orbitrap Mass Spectroscopy

  • 摘要: 建立超高效液相色谱-四极杆/静电场轨道阱质谱(UHPLC-Q/Orbitrap)快速筛查和定量检测食用油脂中天然辣椒素、合成辣椒素和二氢辣椒素的分析方法。结果表明,前处理最佳条件为:样品经二氯甲烷溶解,氢氧化钠水溶液提取,硫酸酸化,PRiME HLB固相萃取小柱净化;液质最佳条件为:0.1%甲酸水-0.1%甲酸乙腈梯度洗脱,Thermo Scientific Accucore Vanquish C18+色谱柱(100 mm×2.1 mm,1.5 μm)分离,静电场轨道阱质谱分析检测。结果表明:3种辣椒素在0.1~40 μg/L范围内线性关系良好,R2≥0.999;3个加标水平(n=6)的平均回收率在66.7%~112.8%范围内,相对标准偏差在3.2%~9.7%范围内;检出限在0.02~0.05 μg/kg之间,定量限在0.1~0.2 μg/kg之间。该方法可在无标准物质的情况下对食用油脂中3种辣椒素进行快速筛查及确证,同时可在有标准物质下进行准确定量,为食用油脂中非法添加回收油脂的筛查确证和准确定量检测提供新的技术和思路。

     

    Abstract: A method was developed for rapid screening of and quantification capsaicin, nonivamide and dihydrocapsaicin in edible oil using ultra-high performance liquid chromatography-quadrupole/orbitrap mass spectrometry (UHPLC-Q/Orbitrap). Samples were dissolved in dichloromethane, and then extracted with sodium hydroxide solution and acidified with sulfuric acid. The extract was cleaned up on a Prime HLB solid phase extraction (SPE) column and separated by UHPLC on Thermo Scientific Accucore Vanquish C18+ (100 mm×2.1 mm, 1.5 μm) column. The mobile phase was acetonitrile containing 0.1% formic acid and water containing 0.1% formic acid with gradient elution. Data were collected by Q/Orbitrap MS. The results showed that good linearity was observed in the concentration range from 0.1 to 40 μg/L for all 3 capsaicinoid, with absolute coefficients (R2) greater than 0.999. The average recoveries were in the range from 66.7% to 112.8% at 3 spiked levels with relative standards deviation (RSDs) between 3.2% and 9.7%. The limits of detection (LODs) ranged from 0.02 to 0.05 μg/kg and limit of quantitation between 0.1 to 0.2 μg/kg. The method can quickly screen and confirm three capsaicins in edible oils without reference materials, and can also accurately quantify with reference materials, providing new technologies and ideas for screening confirmation and accurate quantification of illegally added recycled fats in edible oils.

     

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