基于TiO_(2)/KCC-1固相萃取的亲水作用超高效液相色谱-串联质谱法测定南极磷虾磷脂  

Determination of Phospholipids in Antarctic Krill by Hydrophilic Interaction Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry Using TiO_2/KCC-1 Solid Phase Extraction

作　　者：张欣彤 唐光治 沈清 雷敏 谭舒萍 林碧玲 周瑞淇 梁秀碧 郭莲仙 李林秋 ZHANG Xintong;TANG Guangzhi;SHEN Qing;LEI Min;TAN Shuping;LIN Biling;ZHOU Ruiqi;LIANG Xiubi;GUO Lianxian;LI Linqiu(The Public Service Platform of South China Sea for R&D Marine Biomedicine Resources,Marine Biomedical Research Institute,Guangdong Medical University,Zhanjiang 524023,China;Dongguan Key Laboratory of Public Health Laboratory Science,School of Public Health,Guangdong Medical University,Dongguan 523808,China;Institute of Seafood,Zhejiang Gongshang University,Hangzhou 310012,China;Shanghai AB Sciex Analytical Instrument Trading Co.Ltd.,Shanghai 200335,China)

机构地区：[1]广东医科大学海洋医药研究院南海海洋生物医药资源研发公共服务平台,广东湛江524023 [2]广东医科大学公共卫生学院,东莞市卫生检验与检疫重点实验室,广东东莞523808 [3]浙江工商大学海洋食品研究院,浙江杭州310012 [4]上海爱博才思分析仪器贸易有限公司,上海200335

出　　处：《食品科学》2024年第15期168-177,共10页Food Science

基　　金：东莞市社会发展科技项目(20231800939972);东莞市科技特派员项目(20221800500752);广东省医学科研基金项目(A2021036)。

摘　　要：以自制钛基树枝状纤维形SiO_(2)(TiO_(2)/KCC-1)纳米材料作为固相萃取(solid phase extraction,SPE)填料对南极磷虾中的磷脂进行纯化,采用亲水色谱柱结合超高效液相色谱串联质谱法进行磷脂组学分析。选取南极磷虾中最主要的4类磷脂(磷脂酰胆碱(phosphatidylcholines,PC)、磷脂酰乙醇胺(phosphatidyl ethanolamine,PE)、磷脂酰丝氨酸(phosphatidylserine,PS)、磷脂酰肌醇(phosphatidylinositol,PI))作为研究对象。结果显示,在最优条件下共检测到291种磷脂,比已报道的方法多近1倍。在这些磷脂中,含有单不饱和脂肪酸链的磷脂占总磷脂含量的54.73%,含有多不饱和脂肪酸链的磷脂占总磷脂含量的26.17%。南极磷虾中共检出PC 75种、PE 120种、PI 54种、PS 42种。其中PC(40:6)(41.63%)、PE(36:0)(39.77%)、PI(38:3)(80.05%)、PS(36:1)(81.62%)在4类磷脂中的含量最高。多元统计分析结果显示,SPE处理前后磷脂种类有明显差异,Ti O_(2)/KCC-1材料对磷脂的富集效果显著,特别是对PC(18:0/18:0)、PE(16:0/18:1)、PI(16:0/18:2)等富集作用明显。PC、PE和PS的检出限均为0.05μg/g,PI的检出限为0.01μg/g,4种磷脂的相对标准偏差在0.89%~5.05%之间,回收率在87%~112%之间。该方法专一性强、提取效率高、灵敏度和精密度高、准确度好,在生物样本中磷脂的提取、纯化及其检测方面具有广阔的应用前景。Phosphatidylcholine (PC),phosphatidyl ethanolamine (PE),phosphatidylserine (PS),and phosphatidylinositol(PI) are the four major phospholipids in Antarctic krill.In this study,the composition of these phospholipids was analyzed by hydrophilic interaction ultra-high performance liquid chromatography-tandem mass spectrometry (HILIC-UPLC-MS/MS) after purification by solid-phase extraction (SPE) using titania-coated fibrous silica (TiO_2/KCC-1) nanoparticles,which had been prepared in our laboratory.The results showed that under the optimal conditions,291 phospholipids including 75PCs,120 PEs,54 PIs and 42 PSs were detected,which were nearly twice as many as those detected by a previously reported method.Phospholipids containing monounsaturated and polyunsaturated fatty acid chains accounted for 54.73%and 26.17%of the total phospholipids,respectively.PC (40:6)(41.63%),PE (36:0)(39.77%),PI (38:3)(80.05%),and PS (36:1)(81.62%)were found to be the most abundant in the four phospholipids.Multivariate statistical analysis showed significant differences in the types of phospholipids before and after SPE treatment.TiO_2/KCC-1 nanoparticles exhibited a significant enrichment capacity for phospholipids,especially PC (18:0/18:0),PE (16:0/18:1),and PI (16:0/18:2).The detection limit was 0.05 μg/g for PC,PE and PS,and 0.01 μg/g for PI.The relative standard deviations (RSDs) for the four major phospholipids were in the range of 0.89%to 5.05%,and the recoveries were 87%–112%.This method demonstrated high specificity,extraction efficiency,sensitivity,precision and accuracy.Therefore,it has broad application prospects for the extraction,purification,and analysis of phospholipids in biological samples.

关 键 词：钛基树枝状纤维形SiO_(2) 固相萃取 亲水作用超高效液相色谱-串联质谱法 南极磷虾 磷脂 

分 类 号：O657.63[理学—分析化学]