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| 超高效液相色谱-三重四极杆串联质谱法同时
测定植物油中4种维生素E异构体 |
| Simultaneous determination of four vitamin E isomers in vegetable oil by ultra-high performance liquid chromatography- triple quadrupole tandem mass spectrometry |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.230358 |
| 中文关键词: 维生素E 植物油 超高效液相色谱-三重四极杆串联质谱 |
| 英文关键词:vitamin E vegetable oil UPLC-MS/MS |
| 基金项目:未来食品技术创新中心建设项目资金(BM2020023) |
| Author Name | Affiliation | | LI Cailing1, ZHANG Jian1,2, LIU Yuanfa1,3, WANG Xiaochao1, MEI Dongxu1 | （1.Future Food (Bai Ma) Research Institute, Nanjing 210000，China
2.Nanjing Fuzhe Future Food
Research Institute Co. , Ltd. , Nanjing 210000, China
3.School of Food Science and Technology, Jiangnan
University, Wuxi 214122, Jiangsu, China） |
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| 中文摘要: |
| 为提高植物油中4种维生素E异构体（α-、β-、γ-、δ-生育酚）的检测效率，建立一种超高效液相色谱-三重四极杆串联质谱法（UPLC-MS/MS）同时测定植物油中4种维生素E异构体含量的方法。分别对质谱条件、色谱条件及样品前处理条件进行了优化，并对检测方法进行了考察。结果表明：0.5 g样品经10 mL甲醇提取，35 mg C18粉末净化后，采用Kintex F5色谱柱（2.1 mm × 100 mm，1.7 μm）分离，以0.1%甲酸水溶液和0.1%甲酸-甲醇溶液为流动相梯度洗脱，流速0.4 mL/min,电喷雾离子源在正离子模式下进行多反应监测扫描，采用外标法对4种维生素E异构体进行定量；在该条件下，4种维生素E异构体在1～100 ng/mL质量浓度范围内线性关系良好，相关系数（R2）均在0.998以上，检出限均为6 ng/g，定量限均为20 ng/g，加标回收率范围为92.0%～108.0%，相对标准偏差为0.7%～7.1%,与国标方法测定结果相对误差在-4.3%~5.1%。该方法准确、灵敏、重现性好，可应用于实际样品的分析。 |
| 英文摘要: |
| To improve the detection efficiency of four vitamin E isomers (α-, β-, γ-, δ - tocopherol) in vegetable oil, a method for simultaneous determination of the content of four vitamin E isomers (α-, β-, γ-, δ - tocopherol) in vegetable oil by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS) was established. The conditions of mass spectrometry, chromatography, and sample pretreatment were optimized, and the method established was examined. The results showed that the sample (0.5 g) was extracted with methanol(10 mL), purified with C18 powder （35 mg）, separated with Kintex F5 chromatographic column (2.1 mm×100 mm, 1.7 μm), eluted with 0.1% formic acid aqueous solution and 0.1% formic acid-methanol solution as mobile phase by gradient under the speed of 0.4 mL/min, detected under positive ion mode of electric spray (ESI) and multi reaction monitoring mode (MRM), and quantified by external standard method. Under these conditions, there were a good linear relationships for four vitamin E isomers in the mass concentration range of 1-100 ng/mL, with correlation coefficients (R2) above 0.998, detection limits of 6 ng/g, and quantification limits of 20 ng/g. The recovery rate ranged from 92.0% to 108.0%, the relative standard deviation was 0.7%-7.1%, and the relative error of the determination results with national standard method was -4.3%-5.1%. This method has the advantages of accuracy, sensitivity, and good reproducibility, and it can be applied to the analysis of actual samples. |
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