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| Determination of oxalic acid in sesame seed and sesame paste by high performance liquid chromatography |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.230614 |
| KeyWord:HPLC sesame seed sesame paste oxalic acid quantitative detection |
| FundProject: |
| Author Name | Affiliation | | WANG Danyang1, WU Zhenzhen2, SHI Haiming2,
AN Hongzhou1, JIANG Yuanrong1,2 | 1.Colloge of Food Science and Engineering, Henan University of Technology, Zhengzhou 450001, China
2.Wilmar Biotechnology Research and Development Center (Shanghai) Co., Ltd., Shanghai 200137, China |
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| Abstract: |
| Aiming to provide reference for the development of oxalic acid detection methods in sesame seed and sesame products, a high performance liquid chromatography method was established to determine the content of oxalic acid in sesame seed and sesame paste. The extraction conditions for oxalic acid and liquid chromatography conditions were optimized, and the methodology was validated. The oxalic acid content in actual samples was also determined. The results showed that the optimal oxalic acid extraction conditions were as follows: extraction by heating in an 80 ℃ water bath, 1.0 mol/L hydrochloric acid solution as extraction solution, material to liquid ratio 1∶ 10, extraction times twice, and each extraction time 10 min.The optimized liquid chromatography conditions were an Agilent Zorbax SB-Aq column (4.6 mm× 250 mm, 5 μm), with a mobile phase of 0.1% phosphoric acid solution and a flow rate of 0.5 mL/min. Under the optimal chromatography conditions, oxalic acid exhibited a good linear relationship (r2≥0.999 0) within the mass concentration range of 10-2 000 μg/mL. The detection limit and quantification limit of the method were 0.083 mg/g and 0.250 mg/g(based on the mass of defatted sample), respectively. The relative standard deviation of both intra-and inter-day precision were less than 1%. The spiked recovery rates in defatted sesame seed and sesame paste samples were 94.4%-107.5%, and 90.9%-99.7%, respectively. The oxalic acid content in sesame seed was 12.12-24.15 mg/g, and the oxalic acid content in sesame paste was 17.59-25.35 mg/g. In conclusion, the established method has good precision and high accuracy, and can be applied to the detection of oxalic acid content in sesame seed and sesame paste. |
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