采用 LC-MS/MS 分析母乳中的维生素 D-硫酸盐和 25-羟基维生素 D-硫酸盐。
Analysis of vitamin D-sulfate and 25-hydroxyvitamin D-sulfate in breastmilk by LC-MS/MS.
机构信息
Mayo Clinic Department of Physiology & Biomedical Engineering, 200 First St. SW, Rochester, MN 55905 USA.
Mayo Clinic Department of Laboratory Medicine & Pathology, 200 First St. SW, Rochester, MN 55905 USA.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Jan 1;1232:123954. doi: 10.1016/j.jchromb.2023.123954. Epub 2023 Dec 6.
Sulfated metabolites of vitamin D have been suggested to be in breastmilk, although current methods to measure sulfated vitamin D compounds in breastmilk by liquid chromatography-tandem mass spectrometry (LC-MS/MS) have not adequately accounted for increased aqueous solubility of these sulfated metabolites. The purpose of this study was to generate a method of LC-MS/MS for measuring vitamin D-3-sulfate (VitD-S) and 25-hydroxyvitamin D-3-sulfate (25OHD-S) specifically in human breastmilk. The resulting method uses methanol to precipitate protein and solid phase extraction to prepare the samples for LC-MS/MS. The limits of quantification for analytes in solvent were 0.23 ng/mL VitD-S and 0.2 ng/mL 25OHD-S. Various experiments observed concentrations ranging 0.53 to 1.7 ng/mL VitD-S and ≤ 0.29 ng/mL 25OHD-S. Both analytes were present in aqueous skim milk, demonstrating the enhanced aqueous solubility of these vitamin D sulfates. In conclusion, we describe an effective method for measuring VitD-S and 25OHD-S in breastmilk by LC-MS/MS.
已有人提出，维生素 D 的硫酸代谢物存在于母乳中，尽管目前通过液相色谱-串联质谱（LC-MS/MS）测量母乳中硫酸维生素 D 化合物的方法并未充分考虑到这些硫酸代谢物的水溶性增加。本研究的目的是生成一种专门用于测量人乳中维生素 D-3-硫酸盐（VitD-S）和 25-羟维生素 D-3-硫酸盐（25OHD-S）的 LC-MS/MS 方法。该方法使用甲醇沉淀蛋白，固相萃取（SPE）对样品进行 LC-MS/MS 前处理。溶剂中分析物的定量下限分别为 0.23ng/mL VitD-S 和 0.2ng/mL 25OHD-S。各种实验观察到 VitD-S 的浓度范围为 0.53 至 1.7ng/mL，25OHD-S 的浓度范围为≤0.29ng/mL。两种分析物均存在于水脱脂牛奶中，这表明这些维生素 D 硫酸盐的水溶性增强。总之，我们描述了一种通过 LC-MS/MS 有效测量母乳中 VitD-S 和 25OHD-S 的方法。
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