| 阳曦1，向世杰2.固相萃取-液相色谱-串联质谱法测定食用油脂中的合成辣椒素、天然辣椒素和二氢辣椒素[J].中国油脂,2021,46(5):.[YANG Xi1, XIANG Shijie2.Determination of synthetic capsaicin, natural capsaicin and dihydrocapsaicin in edible oil by solid phase extraction-liquid chromatography-tandem mass spectrometry[J].China Oils and Fats,2021,46(5):.] |
| 固相萃取-液相色谱-串联质谱法测定食用油脂中的合成辣椒素、天然辣椒素和二氢辣椒素 |
| Determination of synthetic capsaicin, natural capsaicin and dihydrocapsaicin in edible oil by solid phase extraction-liquid chromatography-tandem mass spectrometry |
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| DOI： |
| 中文关键词: 关键词：固相萃取 液相色谱-串联质谱法 辣椒素 食用油脂 餐厨废油 |
| 英文关键词:Key words：solid phase extraction liquid chromatography-tandem mass spectrometry capsaicinoids edible oil kitchen waste oil |
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| 中文摘要: |
| 摘要：建立了食用油脂中天然辣椒素、合成辣椒素和二氢辣椒素的固相萃取-液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经2%氢氧化钠溶液提取，C18固相萃取小柱净化后，进高效液相色谱-串联质谱仪，采用乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱，多反应监测（MRM）在正离子模式下进行质谱扫描，对3种辣椒素进行定量测定。结果表明，合成辣椒素、天然辣椒素和二氢辣椒素在0.5~50 ng/mL质量浓度范围线性关系良好，相关系数大于0.999 0，三者检出限分别为0.05、0.03、0.03 μg/kg，回收率在71.2%~87.5%之间，相对标准偏差小于4.0%。该方法快速、准确，灵敏度高，能有效满足实验室对食用油脂中非法添加餐厨废油的定量检测。 |
| 英文摘要: |
| Abstract：A rapid determination method of synthetic capsaicin, natural capsaicin and dihydrocapsaicin in edible oil by solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS) was established. The samples were extracted by 2% sodium hydroxide solution, purified with C18 solid phase extraction column, then injected into high performance liquid chromatography-tandem mass spectrometry for quantitative determination of three capsaicinoids using acetonitrile and 0.1% formic acid aqueous solution as the mobile phase for gradient elution and multiple reaction monitoring (MRM) to scan mass spectrometry in positive ion mode.The results showed that the linear relationships of synthetic capsaicin, natural capsaicin and dihydrocapsaicin were good in the range of 0.5-50 ng/mL, and the correlation coefficients were all greater than 0.999 0,the detection limits were 0.05, 0.03 μg/kg and 0.03 μg/kg respectively, the recoveries were 71.2%-87.5%, and the relative standard deviations were less than 4.0%. The method was rapid, accurate and sensitive, and could effectively meet the laboratory quantitative determination of illegal addition of kitchen waste oil in edible oil. |
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