基于单分散微球的固定化金属亲和色谱法制备南极磷虾磷脂，然后进行 HILIC-MS 分析。
Monodisperse microsphere-based immobilized metal affinity chromatography approach for preparing Antarctic krill phospholipids followed by HILIC-MS analysis.
机构信息
Zhejiang Province Key Laboratory of Anesthesiology, The Second Affiliated Hospital and Yuying Children's Hospital of Wenzhou Medical University, Wenzhou, China; Collaborative Innovation Center of Seafood Deep Processing, Zhejiang Province Joint Key Laboratory of Aquatic Products Processing, Institute of Seafood, Zhejiang Gongshang University, Hangzhou, China.
Zhejiang Provincial Key Laboratory of Advanced Mass Spectrometry and Molecular Analysis, Institute of Mass Spectrometry, Ningbo University, Ningbo, Zhejiang 315211, China.
出版信息
Food Chem. 2021 May 15;344:128585. doi: 10.1016/j.foodchem.2020.128585. Epub 2020 Nov 9.
Phospholipids enriched krill is a functional food beneficial in cardiovascular diseases. Herein, monodisperse microsphere-based immobilized metal affinity chromatographic material (MM-IMAC) was synthesized with Ti incorporated to enrich phospholipids from krill by coordination with phosphate group. The extract was profiled by hydrophilic interaction chromatography-mass spectrometry (HILIC-MS) with 154 phospholipid molecular species detected. The parameters were loading solvent n-hexane/isopropanol (2:8, v/v), flow rate 0.8 mL·min, and eluting volume 1 mL. Besides, eicosapentaenoic and docosahexaenoic acids structured phospholipids were located, such as phosphatidylcholine (PC) 20:5/22:6, phosphatidylinositol (PI) 18:0/20:5, etc. Finally, this method was validated in linearity (R ≥ 0.9953), sensitivity (LOD ≤ 0.53 μg·mL and LOQ ≤ 1.66 μg·mL), precision (RSD ≤ 4.86% and RSD ≤ 6.25%), and recovery (58-83%). It indicated that the MM-Ti-IMAC-HILIC-MS was reliable and efficient in specific study of phospholipids in food matrix.
富含磷脂的磷虾是一种有益于心血管疾病的功能性食品。在此，通过与磷酸基团的配位，合成了一种具有 Ti 掺入的单分散微球固定化金属亲和色谱材料 (MM-Ti-IMAC)，用于从磷虾中富集磷脂。通过亲水作用色谱-质谱联用 (HILIC-MS) 对提取物进行了分析，共检测到 154 种磷脂分子种类。参数为上样溶剂正己烷/异丙醇（2:8，v/v），流速 0.8 mL·min，洗脱体积 1 mL。此外，还定位了二十碳五烯酸和二十二碳六烯酸结构磷脂，如磷脂酰胆碱 (PC) 20:5/22:6、磷脂酰肌醇 (PI) 18:0/20:5 等。最后，该方法在线性（R ≥ 0.9953）、灵敏度（LOD ≤ 0.53 μg·mL 和 LOQ ≤ 1.66 μg·mL）、精密度（RSD ≤ 4.86% 和 RSD ≤ 6.25%）和回收率（58-83%）方面进行了验证。结果表明，MM-Ti-IMAC-HILIC-MS 可用于食品基质中特定磷脂的可靠和高效研究。
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