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| Optimization of the method for determination of 3-chloro-1,2-propanediol by adenine pre-column derivatization-HPLC-FLD |
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| DOI：10.12166/j.zgyz.1003-7969/2020.08.026 |
| KeyWord:edible oil 3-chloro-l,2-propanediol(3-MCPD) high performance liquid chromatography- fluorescence detection(HPLC-FLD) adenine |
| FundProject:湖北省粮食科技创新项目； 大宗粮油精深加工教育部重点实验室（武汉轻工大学）开放课题(2018JYBQGDKFA02)；国家自然科学基金项目（31371783） |
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| Abstract: |
| The 3-chloro-1,2-propanediol(3-MCPD) was oxidatively cleaved with sodium periodate solution and then derivatized with adenine to produce a strong fluorescent substance of 1, N6-vinylidene adenine (ε-Ade). According to the study of the products fluorescence spectrum and the optimization of important influencing factors, the determination conditions of 3-MCPD by high performance liquid chromatography-fluorescence detection (HPLC-FLD) method was optimized after the suppression of the background interference of the measurement system. The optimal conditions were obtained as follows: an alkaline-resistant reverse-phase C18 column used for determination, the volume fraction of methanol in the mobile phase 20%, and sodium carbonate-sodium bicarbonate buffer solution of pH 9.0 used as the aqueous phase. For the determination of 3-MCPD in edible oil, 0.01 g/mL NaCl solution should be used as the extraction aqueous phase, and the sodium periodate used for oxidative cracking of 3-MCPD was reduced by the same amount of sodium sulfite and finally removed by the precipitation with 1.1 times its amount of lead acetate so as to suppress the interference of the blank peak. The method was applied in the determination of a variety of edible vegetable oil samples, and the results showed that the method was highly accurate and reproducible (RSD was between 0.32% and 4.63%). The edible oil samples chromatography showed that the matrix interference was very low and the selectivity of the method was wonderful. |
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