Quantitative analysis of four tocopherols in edible oils by freezing crystallization-high performance liquid chromatography method
  
DOI:10.19902/j.cnki.zgyz.1003-7969.240322
KeyWord:freeze crystallization method  tocopherol  quantitative analysis  edible oil
FundProject:甘肃省重大专项(21ZD4NK045);云南省重大科技专项(202302AE090007);陇南油橄榄产业创新联合体项目(2022-L·YGL-06)
Author NameAffiliation
QIU Dongqi1,2, ZHAO Yindi1,2, PEI Dong2,3, HUANG Xinyi1,2, DI Duolong1,2 1.College of Pharmacy, Gansu University of Chinese Medicine, Lanzhou 730000, China
2.CAS Key Laboratory of Chemistry of Northwestern Plant Resources & Key Laboratory of Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China
3.Yunnan Olive Health Industry Innovation Research and Development Co. , Ltd. , Lijiang 674100, Yunnan, China 
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Abstract:
      In order to improve the detection efficiency of tocopherols, a method of freezing crystallization-high performance liquid chromatography (HPLC) for the quantitative analysis of four tocopherols, α-, β-, γ- and δ-tocopherols in edible oils was developed, and the method was applied to the quantitative determination of tocopherols in edible oils such as corn oil, peanut oil, and extra virgin olive oil. The results showed that the optimal method was that 1.0 g oils were fully dissolved in 40 mL solvent mixture of methanol-ethyl acetate-ethanol (volume ratio of 5∶ 3∶ 2), and then frozen at -18 ℃ for 24 h. The samples were extracted, filtered, evaporated under vacuum and re-dissolved and then detected. The HPLC was carried out on a C30 column, with the mobile phases of ethanol-isopropanol (volume ratio of 8∶ 1) and water for isocratic elution. The samples were quantified by the external standard method. The linearity of the four tocopherols was good in the mass concentration range of 2-100 μg/mL, the lowest limit of detection was 0.179 μg/mL, and the lowest quantitative limit was 0.59 μg/mL. The relative standard deviations (RSD) of the intra-day and inter-day precision of the method ranged from 0.57% to 4.98% and 1.67% to 4.34%, and the spiked recoveries ranged from 96.57% to 109.14%, respectively. In conclusion, the freezing crystallization-HPLC method is suitable for the quantitative determination of tocopherols in edible oils because of its easy operation, high extraction efficiency and good accuracy.
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