超高效液相色谱-串联四极杆飞行时间高分辨质谱用于太平洋鳕鱼脂质轮廓分析

引用本文: 蓝皓慧, 王昕岑, 张晓梅, 张鸿伟, 丛培旭, 徐杰, 薛长湖. 超高效液相色谱-串联四极杆飞行时间高分辨质谱用于太平洋鳕鱼脂质轮廓分析[J]. 分析化学, 2020, 48(7): 903-911. doi: 10.19756/j.issn.0253-3820.191595 shu

Citation: LAN Hao-Hui, WANG Xin-Cen, ZHANG Xiao-Mei, ZHANG Hong-Wei, CONG Pei-Xu, XU Jie, XUE Chang-Hu. Lipid Profile Analysis Method Based on Ultra High Performance Liquid Chromatography-Triple Time-of-Flight Tandem Mass Spectrometry and Its Application in Gadus Macrocephalus[J]. Chinese Journal of Analytical Chemistry, 2020, 48(7): 903-911. doi: 10.19756/j.issn.0253-3820.191595 shu

超高效液相色谱-串联四极杆飞行时间高分辨质谱用于太平洋鳕鱼脂质轮廓分析

蓝皓慧 ^1, ,
王昕岑 ^1, ,
张晓梅 ^2, ,
张鸿伟 ^2, ,
丛培旭 ^1, ,
徐杰 ^1, ,
薛长湖 ^1,

1.
中国海洋大学食品科学与工程学院, 青岛 266003;
2.
青岛海关技术中心, 青岛 266000
基金项目:
本文系国家重点研发计划专项（No.2018YFD0901101）资助

摘要: 建立了超高效液相色谱-串联四极杆飞行时间高分辨质谱（UPLC-Triple TOF-MS/MS）分析脂质轮廓的方法。色谱柱选用ACQUITY UPLC CSH C₁₈柱（150 mm×2.1 mm，1.7 μm），流动相A为乙腈-水（65：35，V/V），流动相B为异丙醇-乙腈（85：15，V/V），两者均含5 mmol/L甲酸铵和0.1%甲酸；质谱采用IDA自动二级扫描模式。13类脂质标准品在一定浓度范围内具有良好的线性关系，线性相关系数（R²）均大于0.995，检出限（LOD）为0.001~0.25 μmol/L，定量限（LOQ）为0.0025~0.2 μmol/L，相对标准偏差（RSD）均小于10%，大部分标准品的回收率大于80%。采用氯仿-甲醇（2：1，V/V）提取太平洋鳕鱼肌肉组织中的脂质，共鉴定出498个脂质分子种类，包括255个磷脂、52个鞘脂、191个甘油酯，主要亚类分别为磷脂酰乙醇胺、鞘磷脂、甘油二酯。本方法具有高灵敏、高分辨和高通量等优点，可用于太平洋鳕鱼脂质轮廓的分析，为脂质组学在水产品领域中的应用奠定了方法学基础。

关键词:

English

Lipid Profile Analysis Method Based on Ultra High Performance Liquid Chromatography-Triple Time-of-Flight Tandem Mass Spectrometry and Its Application in Gadus Macrocephalus

1.
College of Food Science and Engineering, Ocean University of China, Qingdao 266003, China;
2.
Technology Center of Qingdao Customs District, Qingdao 266000, China
Received Date: 11 October 2019
Revised Date: 27 April 2020
Fund Project:
This work was supported by the National Key R&D Program of China (No. 2018YFD0901101).

Abstract: A method for analysis of lipid profile by ultra high performance liquid chromatography-triple time-of-flight tandem mass spectrometry (UPLC-Triple TOF-MS/MS) was established. The chromatographic column was selected, and the concentration of ammonium formate in mobile phase and the collision energy of mass spectrometry were optimized. The ACQUITY UPLC CSH C₁₈ chromatographic column (150 mm×2.1 mm, 1.7 μm) was used. The mobile phase A was acetonitrile/water (65:35, V/V), the mobile phase B was isopropanol/acetonitrile (85:15, V/V), and both of which contained 5 mmol/L ammonium formate and 0.1% formic acid. IDA automatic secondary scanning mode was adopted for mass spectrometry. Through methodological verification, lipid standards maintained good linearity in certain concentration ranges. The correlation coefficients (R²) were all above 0.995, the limits of detection (LOD) were 0.001-0.25 μmol/L, the limits of quantification (LOQ) were 0.0025-0.2 μmol/L, and the relative standard deviations were less than 10%. Most of the recovery rates were more than 80%. The lipid of Pacific cod (Gadus macrocephalus) was extracted by chloroform-methanol (2:1, V/V). A total of 498 lipid molecular species were identified in Pacific cod, including 255 phospholipid molecular species, 52 sphingolipid molecular species and 191 glyceride molecular species, of which the main subclasses were phosphatidylethanolamine, sphingomyelin and diglyceride. The results showed that the method had high sensitivity, high resolution and high throughput, and could be applied to the analysis of lipid profile of Pacific cod, which laid a foundation for the application of lipidomics in the field of aquatic products.

Key words:

Lipid profile
/ Ultra high performance liquid chromatography-triple time-of-flight tandem mass spectrometry
/ Phospholipids
/ Sphingolipids
/ Gadus macrocephalus

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沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-串联四极杆飞行时间高分辨质谱用于太平洋鳕鱼脂质轮廓分析

English

Lipid Profile Analysis Method Based on Ultra High Performance Liquid Chromatography-Triple Time-of-Flight Tandem Mass Spectrometry and Its Application in Gadus Macrocephalus

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联四极杆飞行时间高分辨质谱用于太平洋鳕鱼脂质轮廓分析

English

Lipid Profile Analysis Method Based on Ultra High Performance Liquid Chromatography-Triple Time-of-Flight Tandem Mass Spectrometry and Its Application in Gadus Macrocephalus

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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