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| 碱性铁氰化钾衍生测定水果中维生素B1含量的方法优化 |
| Optimization of method for determination of vitamin B1 in fruits by alkaline potassium ferricyanide derivation |
| 投稿时间：2026-05-09 修订日期：2026-07-29 |
| DOI： |
| 中文关键词: 维生素B1 超高效液相色谱法 碱性铁氰化钾 衍生化 水果 |
| 英文关键词:Vitamin B1 UPLC Alkaline potassium ferricyanide Derivatization Fruit |
| 基金项目:中国食物成分监测项目 |
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| 中文摘要: |
| 目的 建立超高效液相色谱法测定水果基质中维生素B1含量的分析方法, 并对衍生和萃取条件进行优化。方法 水果中维生素B1经碱性铁氰化钾衍生后, 正丁醇萃取, 采用ACQUITY UPLC BEH C18 (2.1mm×100 mm, 1.7 μm)色谱柱进行分离, 50 mmol/L乙酸钠溶液和乙腈为流动相, 梯度洗脱, 流速为0.25 mL/min, 柱温度为40 ℃, 激发波长375 nm, 发射波长435 nm, 进样体积为1 μL。以色谱保留时间定性, 标准曲线外标法定量。结果 最佳条件下, 维生素B1在质量浓度为0.05~1.00 μg/mL范围内与峰面积呈现良好的线性关系, 相关系数大于0.9998, 方法定量限为0.80 mg/kg, 检出限为0.30 mg/kg。以不同种类的水果为基质, 采用低、中、高三浓度水平进行加标回收试验考察方法的准确度与精密度, 结果表明, 维生素B1的平均回收率为79.6%~112%, 相对标准偏差小于4.7%。结论 将建立的方法用于不同水果样品中维生素B1的测定, 表明该方法的样品前处理简便、快速, 准确度高, 精密度好, 适用于批量水果中维生素B1含量的快速测定。 |
| 英文摘要: |
| Objective To establish a method for the determination of vitamin B1 in fresh fruit matrix by ultra-high performance liquid chromatography and the derivatization and extraction conditions were optimized. Methods Vitamin B1 in fruit samples was derivatized with alkaline potassium ferricyanide and then extracted using n-butanol. Chromatographic separation was performed on an ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm). The mobile phase consisted of 50 mmol/L sodium acetate solution and acetonitrile with gradient elution. The flow rate was set at 0.25 mL/min, and the column temperature was maintained at 40 ℃. The excitation and emission wavelengths were 375 nm and 435 nm, respectively, and the injection volume was 1 μL. Qualitative analysis was conducted based on chromatographic retention time, and quantitative detection was carried out via external standard method with standard curve. Results Vitamin B1 showed a good linear relationship with peak area within the mass concentration range of 0.05-1.00 μg/mL, the correlation coefficient was greater than 0.9998, and the limit of quantitation and limit of detection were 0.80 mg/kg and 0.30 mg/kg, respectively. .The accuracy and precision of the method were investigated by using different kinds of fruits as the substrate with low, medium and high concentration levels. The average recovery of vitamin B1 was 79.6%-112%, and the relative standard deviation was less than 4.7%. Conclusion The established method was applied to the determination of vitamin B1 in various fruit samples. This method features simple and rapid sample pretreatment, high accuracy and favorable precision, and is suitable for the rapid determination of vitamin B1 in large batches of fruit samples. |
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