In a successful fortification program, the stability of micronutrients added to the food is one of the most important factors. The added vitamin D3 is known to sometimes decline during storage of fortified milks, and oxidation through fatty acid lipoxidation could be suspected as the likely cause. Identification of vitamin D3 oxidation products (VDOPs) in natural foods is a challenge due to the low amount of their contents and their possible transformation to other compounds during analysis. The main objective of this study was to find a method to extract VDOPs in simulated whole milk powder and to identify these products using LTQ-ion trap, Q-Exactive Orbitrap and triple quadrupole mass spectrometry. The multistage mass spectrometry (MSⁿ) spectra can help to propose plausible schemes for unknown compounds and their fragmentations. With the growth of combinatorial libraries, mass spectrometry (MS) has become an important analytical technique because of its speed of analysis, sensitivity, and accuracy. This study was focused on identifying the fragmentation rules for some VDOPs by incorporating MS data with in silico calculated MS fragmentation pathways. Diels–Alder derivatization was used to enhance the sensitivity and selectivity for the VDOPs’ identification. Finally, the confirmed PTAD-derivatized target compounds were separated and analyzed using ESI(+)-UHPLC-MS/MS in multiple reaction monitoring (MRM) mode.

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在成功的防御计划中，添加到食物中的微量营养素的稳定性是最重要的因素之一。已知添加的维生素D3在强化牛奶的存储过程中有时会下降，并且可能被怀疑是通过脂肪酸脂氧化引起的氧化。天然食品中维生素D3氧化产物（VDOPs）的鉴定是一项挑战，因为其含量低并且在分析过程中可能转化为其他化合物。这项研究的主要目的是找到一种提取模拟全脂奶粉中VDOP的方法，并使用LTQ离子阱，Q-Exactive Orbitrap和三重四极杆质谱法鉴定这些产品。多级质谱法（MS ⁿ光谱有助于为未知化合物及其碎片化提出合理的方案。随着组合库的增长，质谱（MS）由于其分析速度，灵敏度和准确性而成为一种重要的分析技术。这项研究的重点是通过将质谱数据与计算机计算的质谱碎裂途径相结合，从而确定某些VDOP的碎裂规则。Diels–Alder衍生化用于增强VDOP识别的灵敏度和选择性。最后，将已确认的PTAD衍生的目标化合物分离出来，并使用ESI（+）-UHPLC-MS / MS在多反应监测（MRM）模式下进行分析。

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