| 张方圆.同位素内标-气相色谱-质谱法测定食用植物油中缩水甘油酯[J].中国油脂,2020,45(12):132~136.[ZHANG Fangyuan.Determination of glycidyl esters in edible vegetable oil by isotopic internal standard-gas chromatography-mass spectrometry[J].China Oils and Fats,2020,45(12):132~136.] |
| 同位素内标-气相色谱-质谱法测定食用植物油中缩水甘油酯 |
| Determination of glycidyl esters in edible vegetable oil by isotopic internal standard-gas chromatography-mass spectrometry |
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| DOI：10.12166/j.zgyz.1003-7969/2020.12.025 |
| 中文关键词: 缩水甘油酯 同位素内标 水解 衍生 食用植物油 GC-MS |
| 英文关键词:glycidyl esters isotopic internal hydrolysis derivatization edible vegetable oil GC-MS |
| 基金项目:广东省科学院青年科技工作者引导专项（2019 GDASYL-0105013）；广东省测试分析研究所（中国广州分析测试中心）自筹科研资金项目（201902） |
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| 中文摘要: |
| 建立了一种同位素内标-气相色谱-质谱法测定食用植物油中缩水甘油酯（GEs）的检测方法。先将GEs转化成3-溴-1，2-丙二醇（3-MBPD）单酯，再通过水解、衍生化，然后气相色谱-质谱法测定3-溴-1，2-丙二醇（3-MBPD）含量，并对衍生条件进行优化。结果表明：优化的衍生条件为GEs质量浓度为21.78 μg/mL时，苯硼酸（PBA）用量100 μL，衍生温度50 ℃，衍生时间10 min。该方法在GEs质量浓度为0.021 8~2.178 μg/mL范围内线性关系良好（R=0.999 9），检出限为25 μg/kg，平均加标回收率为91.4%~97.0%，相对标准偏差为4.4%~86%。该方法的可操作性强、重现性好，灵敏度、准确度和精密度均能满足实际工作中食用植物油中GEs的定性定量检测。 |
| 英文摘要: |
| An isotopic internal standard-gas chromatography-mass spectrometry method was established for the determination of glycidyl esters (GEs) in edible vegetable oil. GEs were converted to 3-monobromopropanediol (3-MBPD) monoesters, and then the 3-MBPD content was determined by gas chromatography-mass spectrometry (GC-MS) after hydrolysis and derivatization. The conditions of derivatization were optimized. The results showed that the optimal derivatization conditions were obtained as follows: mass concentration of GEs 21.78 μg/mL， phenylboronic acid(PBA) dosage 100 μL, derivatization temperature 50 ℃, derivatization time 10 min. Good linearity was obtained (R=0.999 9) with the mass concentration of GEs in the range of 0.021 8-2.178 μg/mL. The limit of detection of GEs was 25 μg/kg，and the mean recovery rate of standard addition was 91.4%-97.0% with a relative standard deviation of 4.4%-8.6%. The method was applicable and reproducible with good sensitivity, accuracy and precision, which could be used for qualitative and quantitative determination of GEs in edible vegetable oil in actual work. |
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