【摘要】 以稻米为检测对象，优化 GB 5009.84—2016《食品安全国家标准 食品中维生素 B₁的测定》第一法高效液相色谱法前处理过程，建立稻米中维生素 B₁含量的超高效液相色谱测定方法。采用 Waters Acquity UPLC BHC C₁₈色谱柱 （50 mm×2.1 mm,1.7 μm），在 0.02 ～ 1.00 μg/mL 的质量浓度范围内呈现良好线性关系，相关系数大于 0.999，检出限 （S/N=3）为 0.4 μg/100 g，定量限 （S/N=10） 为 1.3 μg/100 g,3 个浓度水平下加标回收率为 85.0% ～ 98.6%，精密度为 1.5% ～ 4.6%，超高效液相色谱可以很好地对稻米中维生素 B₁进行快速准确定量分析；采用恒温烘箱水解法与高压灭菌锅水解法结果基本一致；稻谷在加工过程中维生素 B₁会有较大的损失。超高效液相色谱检测方法、恒温烘箱水解法及一次性加入乙酸钠溶液中和酸液均能有效缩短检测时间，实现批量检测，大大提高了检测效率。更多还原

【Abstract】 Take the paddy rice as the examination, the sample pre-treatment method of vitamin B₁ content determination by Liquid Chromatography, which is the first method for GB 5009.84—2016 National Standards for Food Safety the determination of vitamin B₁ in food was improved, to develop an Ultra Performance Liquid Chromatography （UPLC） method for the determination of vitamin B₁ in rice. Waters Acquity UPLC BEH C₁₈ （50 mm × 2.1 mm, 1.7 μm） was used, the calibration curves were acquired in the concentration range of0.05-1.00 μg/mL with correlation coeffcients greater than 0.999, the limits of detection and limits of quantitation were 0.4 and 1.3 μg/100 g for rice, the recoveries of the three levels were ranged from 85.0% to 98.6%, and the relative standard deviations between 1.5% to 4.6%, UPLC allows good rapid and accurate quantitative analysis of vitamin B₁ in rice; there was no significant difference between the results of high pressure sterilization and constant temperature oven hydrolysis method; much of vitamin B₁ actually was refined out of the paddy. UPLC detection method, constant temperature oven hydrolysis method and disposable sodium acetate solution neutralization acid solution can effectively shorten the detection time, and greatly improve the detection effciency in order to achieve batch detection.更多还原