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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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