超高效液相色谱法测定乳粉中维生素B1的前处理条件优化

Optimization of pretreatment conditions for determination of vitamin B1 in milk powder by ultra performance liquid chromatography

中文关键词:  维生素B1  婴幼儿配方乳粉  回收率  高温水解  常温水解

英文关键词:vitamin B1  infant formula milk powder  recovery rate  high-temperature hydrolysis  room-temperature hydrolysis

中文摘要:

      目的 优化婴幼儿配方乳粉中维生素B1 (vitamin B1, VB1)的检测方法。方法 利用超高效液相色谱仪测定不同基质样品中VB1的含量, 分析水解冷却时间、水解温度、生产工艺、酶溶液、原料基质对检测结果的影响, 对婴幼儿配方乳粉中VB1检测的前处理进行优化。结果 检测流程准确可靠, 无乳粉基质的VB1标准溶液回收率达到94.3%~102.0%; 水解冷却时间、生产工艺及混合酶溶液对VB1检测结果及回收率均无显著影响(P>0.05); 水解温度与乳粉基质是导致检测结果偏低的关键协同因素, 常温水解的VB1检测结果及回收率显著高于高温水解(P<0.01), 且混合粉在高温水解后回收率显著下降(P<0.05)。结论 优化后的常温水解方法, 省去高压水解操作, 简化了前处理流程, 且加标回收率接近100%, 该方法适用于婴幼儿配方乳粉中VB1的高效批量检测。

英文摘要:

      Objective To optimize the detection method for vitamin B1 (VB1) in infant formula milk powder. Methods The content of VB1 in different matrix samples was determined by ultra performance liquid chromatography. The effects of hydrolysis cooling time, hydrolysis temperature, production process, enzyme solution and raw material matrix on the detection results were analyzed to optimize the pretreatment for VB1 detection in infant formula milk powder. Results The detection process was accurate and reliable, with recovery rates of 94.3% to 102.0% for VB1 standard solutions without milk powder matrix. Hydrolysis cooling time, production process and mixed enzyme solution had no significant effect on VB1 detection results and recovery rate (P>0.05). Hydrolysis temperature and milk powder matrix were key synergistic factors causing lower detection results. VB1 detection results and recovery rate from room-temperature hydrolysis were significantly higher than those from high-temperature hydrolysis (P<0.01). Furthermore, recovery rate of mixed powders decreased significantly after high-temperature hydrolysis (P<0.05). Conclusion The optimized ambient-temperature hydrolysis method eliminates high-pressure hydrolysis operations, simplifies pretreatment procedures and achieves spiked recovery rates approaching 100%. This method is suitable for the efficient batch detection of VB1 in infant formula milk powder.