基于色谱-质谱联用的脂质分析样品前处理技术研究进展

doi:10.3724/SP.J.1123.2019.06023

摘要/Abstract

摘要：

脂质作为细胞膜和亚细胞膜的主要结构成分，在能量来源、细胞信号传导等多种生物学过程中发挥着重要作用。近年来，脂质分析受到越来越多的关注，其中色谱-质谱联用技术在脂质分析中占据主导地位。由于样品基质复杂，样品前处理有富集痕量物质和减少基质干扰的作用，成为脂质分析中的一个关键步骤。该文综述了近年来基于色谱-质谱联用技术的脂质分析中样品前处理技术的研究进展和应用，对各种样品前处理技术进行了阐述和总结。基于液相的萃取方法有液-液萃取和单一有机溶剂萃取。基于固相的萃取方法包括固相萃取和固相微萃取。场辅助萃取方法包括超临界流体萃取、加压流体萃取、微波辅助萃取和超声辅助萃取。此外，还介绍了在线联用样品前处理方法和用于活体分析的样品前处理方法。最后，对基于色谱-质谱联用的脂质分析样品前处理技术存在的问题及发展趋势进行了探讨。样品前处理技术的发展将提高脂质分析的灵敏度、选择性和分析速度。

关键词: 样品前处理, 脂质分析, 色谱-质谱联用

Abstract:

As the main structural components of cellular and sub-cellular membranes, lipids are a major source of energy and play an important role in various biological processes such as cellular signaling. Lipid profiling has attracted increasing attention in recent years, and chromatography-mass spectrometry techniques for lipid profiling occupy a dominant position in this regard. Sample preparation, which aims at enriching trace substances and reducing matrix interferences, is a crucial step in the analysis of lipids for the intricacy of sample matrices. Here, we review recent developments in sample preparation techniques based on chromatography-mass spectrometry and their application to lipid profiling. Various sample preparation techniques are described and summarized. The extraction methods based on liquid phase included liquid-liquid extraction and single organic solvent extraction. The extraction methods based on solid phase involved solid-phase extraction and solid-phase microextraction. The field-assisted extraction methods cover supercritical fluid extraction, pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction. Moreover, online coupling sample preparation methods and sample preparation methods for in vivo lipid analysis are presented. Finally, the problems and trends in sample preparation techniques for lipid profiling based on chromatography-mass spectrometry are discussed. It is believed that efficient development of sample preparation techniques would help improve the sensitivity and selectivity of lipid profiling as well as the analysis speed.

Key words: sample preparation, lipid profiling, chromatography-mass spectrometry

杨吉娜, 刘丹阳, 周婷. 基于色谱-质谱联用的脂质分析样品前处理技术研究进展[J]. 色谱, 2020, 38(1): 74-85.

YANG Jina, LIU Danyang, ZHOU Ting. Recent advances in sample preparation techniques for the lipid profiling based on chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(1): 74-85.

图/表 1

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Extraction method	Sample type	Analytical techniques	Advantages	Disadvantages	References
Extraction methods based on liquid phase
LLE	cell	LC-MS, GC-MS	well-established method	high consumption of toxic organic solvent	[34, 35]
	plasma, serum	LC-MS, GC-MS, SFC-MS	cheap apparatus and solvents	poor selectivity	[36-39]
	tissue	LC-MS, GC-MS, SFC-MS	short extraction time	phase separation can be difficult	[40-42]
	urine	LC-MS	external energy not required		[43]
SOSE	tissue	LC-MS, SFC-MS	easy to perform	toxic organic solvent consumption	[44-46]
	plasma, serum	LC-MS, SFC-MS	short extraction time	poor selectivity	[47-49]
	cell	LC-MS, GC-MS	external energy not required		[50, 51]
	fecal	GC-MS			[52]
Extraction methods based on solid phase
SPE	cell	LC-MS	no increase in temperature	costly SPE cartridges	[53]
	plasma, serum	LC-MS	matrix interference eliminated	toxic organic solvent consumption	[20, 54-56]
	tissue	LC-MS			[57-59]
SPME	cell	LC-MS	low solvent consumption	small extraction capacity	[60]
	tissue	LC-MS	short extraction time		[61]
Field-assisted extraction methods
SFE	dry blood spot	LC-MS	high extraction efficiency	sophisticated to operate	[62]
	plant	LC-MS, GC-MS, SFC-MS	environment friendly	high instrument investment	[63-65]
	oil	GC-MS			[66, 67]
PLE	soy, egg yolk, ox liver, krill oil	LC-MS	automated extraction technique	expensive	[68]
	microorganism	GC-MS	low solvent consumption		[69]
	tissue	LC-MS	short extraction time		[70]
	seed	GC-MS			[71]
MAE	tissue	GC-MS	high extraction efficiency	potential degradation	[72]
	microalgae	LC-MS			[73]
UAE	tissue	GC-MS	low solvent consumption	need external energy	[74]
	plasma	LC-MS	short extraction time	potential degradation	[75]
	microorganism	GC-MS			[76]
Online coupling methods
	plasma, serum	SPE-LC-MS	automation	sophisticated to operate	[77-79]
	cell	SPE-LC-MS	high throughput	high instrument investment	[80]
	whole blood	SFE-SFC-MS	time saving		[81]
	plant	SFE-SFC-MS	less artificial errors and sample loss		[82]
In vivo lipid profiling
	rat blood	LC-MS	real-time monitoring	difficult to operate	[83]

Extraction method	Sample type	Analytical techniques	Advantages	Disadvantages	References
Extraction methods based on liquid phase
LLE	cell	LC-MS, GC-MS	well-established method	high consumption of toxic organic solvent	[34, 35]
	plasma, serum	LC-MS, GC-MS, SFC-MS	cheap apparatus and solvents	poor selectivity	[36-39]
	tissue	LC-MS, GC-MS, SFC-MS	short extraction time	phase separation can be difficult	[40-42]
	urine	LC-MS	external energy not required		[43]
SOSE	tissue	LC-MS, SFC-MS	easy to perform	toxic organic solvent consumption	[44-46]
	plasma, serum	LC-MS, SFC-MS	short extraction time	poor selectivity	[47-49]
	cell	LC-MS, GC-MS	external energy not required		[50, 51]
	fecal	GC-MS			[52]
Extraction methods based on solid phase
SPE	cell	LC-MS	no increase in temperature	costly SPE cartridges	[53]
	plasma, serum	LC-MS	matrix interference eliminated	toxic organic solvent consumption	[20, 54-56]
	tissue	LC-MS			[57-59]
SPME	cell	LC-MS	low solvent consumption	small extraction capacity	[60]
	tissue	LC-MS	short extraction time		[61]
Field-assisted extraction methods
SFE	dry blood spot	LC-MS	high extraction efficiency	sophisticated to operate	[62]
	plant	LC-MS, GC-MS, SFC-MS	environment friendly	high instrument investment	[63-65]
	oil	GC-MS			[66, 67]
PLE	soy, egg yolk, ox liver, krill oil	LC-MS	automated extraction technique	expensive	[68]
	microorganism	GC-MS	low solvent consumption		[69]
	tissue	LC-MS	short extraction time		[70]
	seed	GC-MS			[71]
MAE	tissue	GC-MS	high extraction efficiency	potential degradation	[72]
	microalgae	LC-MS			[73]
UAE	tissue	GC-MS	low solvent consumption	need external energy	[74]
	plasma	LC-MS	short extraction time	potential degradation	[75]
	microorganism	GC-MS			[76]
Online coupling methods
	plasma, serum	SPE-LC-MS	automation	sophisticated to operate	[77-79]
	cell	SPE-LC-MS	high throughput	high instrument investment	[80]
	whole blood	SFE-SFC-MS	time saving		[81]
	plant	SFE-SFC-MS	less artificial errors and sample loss		[82]
In vivo lipid profiling
	rat blood	LC-MS	real-time monitoring	difficult to operate	[83]

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