在线样品制备技术耦合液相色谱-质谱系统在食品危害物检测中的应用进展

doi:10.3724/SP.J.1123.2023.04026

色谱 ›› 2023, Vol. 41 ›› Issue (12): 1062-1072.DOI: 10.3724/SP.J.1123.2023.04026

在线样品制备技术耦合液相色谱-质谱系统在食品危害物检测中的应用进展

翟洪稳, 马红玉, 曹梅荣, 张明星, 马俊美, 张岩(), 李强^*⁽⁾

河北省食品检验研究院,河北省食品安全重点实验室,国家市场监管重点实验室(特殊食品监管技术),特殊食品安全与健康河北省工程研究中心,河北石家庄 050227

收稿日期:2023-05-05 出版日期:2023-12-08 发布日期:2023-12-13
通讯作者: *E-mail:snowwinglv@126.com(张岩); E-mail:sjzliq@163.com(李强).
基金资助:
河北省市场监督管理局科研计划项目(2021ZD17);国家市场监督管理总局科技计划项目(2020MK014);河北省高层次人才资助项目(A202101055);河北省高层次人才资助项目(C20221051)

Application progress of on-line sample preparation techniques coupled with liquid chromatography-mass spectrometry system in the detection of food hazards

ZHAI Hongwen, MA Hongyu, CAO Meirong, ZHANG Mingxing, MA Junmei, ZHANG Yan(), LI Qiang^*⁽⁾

Hebei Food Safety Key Laboratory, Key Laboratory of Special Food Supervision Technology for State Market Regulation, Hebei Engineering Research Center for Special Food Safety and Health, Hebei Food Inspection and Research Institute, Shijiazhuang 050227, China

Received:2023-05-05 Online:2023-12-08 Published:2023-12-13
Supported by:
Research Project of Hebei Administration for Market Regulation(2021ZD17);Science and Technology Project of State Administration for Market Regulation(2020MK014);Hebei Province High Level Talent Funding Program(A202101055);Hebei Province High Level Talent Funding Program(C20221051)

摘要/Abstract

摘要：

食品安全检测具有重要意义,但食品样品基质复杂,测定其中危害物时,通常需要以下几个步骤:样品制备,即采用适合的样品前处理方法,在不同基质中将目标物分离出来;分离纯化,利用色谱系统进一步分离纯化目标物;定性定量分析,基于目标化合物的性质选择合适的检测器进行分析。其中样品制备是关键步骤之一,将样品制备过程与液相色谱系统耦合可以实现样品的在线自动化分析。与传统人工处理过程相比,在线分析不仅能够减少人工操作误差,保证良好的精密度和重复性,而且可以降低溶剂消耗,避免样品间交叉污染,同时节约分析时间,提高检测效率。本文主要介绍目前常用的在线样品制备技术,包括在线固相萃取(on-line SPE)、管内固相微萃取(in-tube SPME)、湍流色谱法(TFC),详细阐述了其基本原理和耦合设备。在线样品制备技术耦合液相色谱-质谱系统分为两个维度,主要依赖于阀切换技术,将样品制备(第一维度)和液相色谱系统(第二维度)之间建立物理连接,随后采用相应的检测器进行分析。第一维度的作用主要是去除样品杂质,净化分离目标物,为第二维度对目标物进行定性定量检测做准备。此外,文章对3种在线净化系统适用的不同净化填料进行了总结讨论。最后综述了近10年来3类在线系统在食品兽药残留、农药残留、毒素污染以及其他危害物检测中的应用和研究进展,并对该领域存在的问题和发展趋势进行了探讨和展望,以促进在线样品制备技术进一步应用于食品安全检测。

关键词: 在线样品制备技术, 在线固相萃取, 管内固相微萃取, 湍流色谱法, 食品危害物, 综述

Abstract:

Food safety has received increased attention, and food detection is of great significance. The food matrix is complex, and diverse food hazards have been identified. Thus, the detection methods and sample preparation techniques for food matrices must be continuously optimized and updated. Several steps are usually required when a chromatographic system is used to determine food hazards: sample preparation, that is, the separation of targets from different substrates using a suitable preprocessing method and target-substance separation and purification, which is usually achieved using chromatographic separation. The selection of an appropriate detector for qualitative and quantitative analyses is usually based on the properties of the target compound. The sample preparation procedure is considered the most time-consuming aspect of the entire food-analysis process. It is also prone to analytical errors. Therefore, optimization of the sample preparation process is a key issue in the field of chemical analysis. Researchers have developed a series of new, efficient, and accurate sample preprocessing methods, and an on-line sample-preparation system has been found to be a feasible approach. On-line sample preparation coupled with liquid chromatography-mass spectrometry (LC-MS) presents many advantages. First, manual operation could reduce analytical errors to ensure good accuracy and repeatability. It could also reduce the consumption of chemical reagents and avoid cross-contamination between samples. Furthermore, an on-line sample-preparation system could shorten the sample-preparation time and improve the detection efficiency. On-line sample preparation coupled with LC-MS has been widely applied in the fields of environment, biology, and food. On-line sample preparation systems coupled with LC-MS are divided into two modules: the first modules involves sample preparation and the second module involves the LC system. The first module remove impurities and isolates the target compounds in preparation for their qualitative and quantitative detection. The coupling of these two modules depends mainly on valve switching.
In this paper, we introduce the most frequently used on-line sample-preparation techniques, including on-line solid phase extraction (on-line SPE), in-tube solid phase microextraction (in-tube SPME), and turbulent chromatography (TFC). We then describe the basic principles and coupling equipment of these three on-line analytical technologies in detail. The coupling equipment establishes a physical connection between the two modules. Next, we discuss the properties of different purification fillers in an on-line sample-preparation column. The applications and research progress of on-line systems for pesticide residues, veterinary drug residues, and biotoxins are also discussed. Compared with offline sample preparation, on-line analytical systems present several advantages. On-line analytical systems can not only greatly reduce the analysis time and solvent consumption but also improve the detection sensitivity and accuracy. Such systems can be used to determine food hazards to ensure food safety. Finally, the existing problems and development trends of on-line analytical systems are discussed and prospected. To promote the applications of on-line analytical technology in food-safety detection, we suggest that the following three aspects be considered. First, more on-line purification columns with novel fillers, in addition to C18 or polymer fillers, should be developed. Second, compared with ordinary detectors, high-resolution MS detectors have better precision and accuracy. Coupling on-line analytical technologies with a high-resolution mass spectrometer may be beneficial for the further development of on-line analyses. Third, different food matrices should be compared and evaluated to continuously optimize the detection process and improve the efficiency of on-line analytical systems. As concerns regarding food safety issues have increased, the applications of on-line analytical technologies for food detection can be expected to become increasingly important.

Key words: on-line sample preparation techniques, on-line solid phase extraction (on-line SPE), in-tube solid phase microextraction (in-tube SPME), turbulent flow chromatography (TFC), food hazards, review

中图分类号:

O658

翟洪稳, 马红玉, 曹梅荣, 张明星, 马俊美, 张岩, 李强. 在线样品制备技术耦合液相色谱-质谱系统在食品危害物检测中的应用进展[J]. 色谱, 2023, 41(12): 1062-1072.

ZHAI Hongwen, MA Hongyu, CAO Meirong, ZHANG Mingxing, MA Junmei, ZHANG Yan, LI Qiang. Application progress of on-line sample preparation techniques coupled with liquid chromatography-mass spectrometry system in the detection of food hazards[J]. Chinese Journal of Chromatography, 2023, 41(12): 1062-1072.

图/表 7

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Analytes	Matrices	First dimension	Second dimension	On-line analysis system	LODs/ (ng/kg)	LOQs/ (ng/kg)	Recov- eries/%	RSDs/ %	Ref.
10 β-agonists	pork and lamb	MCX column (10 mm×1 mm)	XBridge C18 column (150 mm×4.6 mm, 5 μm)	SPE-UHPLC- MS/MS	4-40	20-200	76.5- 107.7	2.4- 9.5	[15]
18 sulfonamide antibiotics	aquaculture	Oasis^® MCX column (20 mm×2.1 mm, 2.5 μm) and Oasis^® HLB column (20 mm ×2.1 mm, 2.5 μm)	F5 column (150 mm× 3.0 mm, 2.6 μm)	SPE-UHPLC-MS/MS	1.46-15.5	49-51.6	71.5- 102.0	3.47- 14.2	[44]
10 macrolide antibiotics	pork	HLB column (10 mm×1 mm)	XBridge C18 column (100 mm×2.1 mm mm, 2.5 μm)	SPE-UHPLC-MS/MS	50-300	100-1000	69.9- 115.2	0.9- 9.2	[45]
Abamectin and ivermectin	milk	SB-C18 column (30 mm×2.1 mm, 3.5 μm)	SB-C18 column (75 mm×2.1 mm, 3.5 μm)	SPE-UHPLC- MS/MS	0.65-0.67	2.21-2.23	82-88	4.8- 9.7	[46]
36 antibiotics	chicken meat	TurboFlow Cyclone- P (50 mm×0.5 mm, 60 μm)	Betasil phenyl hexyl column (50 mm×2.1 mm, 3 μm)	TFC-HPLC- MS/MS	300-40000	1000-120000	80-120	3-28	[47]
Ractopamine	beef	TurboFlow Cyclone- P (50 mm×0.5 mm, 60 μm)	Accucore C18 column (50 mm×3 mm, 2.6 μm)	TFC-HPLC- MS/MS	-	0.3	85-104	2.6- 14.0	[48]
5 benzimidazoles and 7 metabolites	milk	ADS column (25 mm ×4 mm, 25 μm)	Zorbax Eclipse XDB- C18 column (150 mm ×4.60 mm, 3 μm)	SPE-UHPLC- MS/MS	0.1-0.8	-	88-114	0.8- 9.7	[49]
8 quinolone antibacterials	milk, egg, chicken and fish	PEEK tube (poly (MAA-co-EGDMA), 150 mm×0.50 mm)	C18 column (250 mm ×2.0 mm, 5 μm)	In-tube SPME- LC/ESI-Q- TOF-MS	0.3-1.2 (egg), 0.2-3.0 (milk), 0.2-0.7 (chick- en), 0.2-1.0 (fish)	1.0-4.0 (egg), 0.6-10 (milk), 0.8-2.4 (chick- en), 0.6-3.3 (fish)	80.2- 115.0	1.3- 14.5	[50]

Analytes	Matrices	First dimension	Second dimension	On-line analysis system	LODs/ (ng/kg)	LOQs/ (ng/kg)	Recov- eries/%	RSDs/ %	Ref.
10 β-agonists	pork and lamb	MCX column (10 mm×1 mm)	XBridge C18 column (150 mm×4.6 mm, 5 μm)	SPE-UHPLC- MS/MS	4-40	20-200	76.5- 107.7	2.4- 9.5	[15]
18 sulfonamide antibiotics	aquaculture	Oasis^® MCX column (20 mm×2.1 mm, 2.5 μm) and Oasis^® HLB column (20 mm ×2.1 mm, 2.5 μm)	F5 column (150 mm× 3.0 mm, 2.6 μm)	SPE-UHPLC-MS/MS	1.46-15.5	49-51.6	71.5- 102.0	3.47- 14.2	[44]
10 macrolide antibiotics	pork	HLB column (10 mm×1 mm)	XBridge C18 column (100 mm×2.1 mm mm, 2.5 μm)	SPE-UHPLC-MS/MS	50-300	100-1000	69.9- 115.2	0.9- 9.2	[45]
Abamectin and ivermectin	milk	SB-C18 column (30 mm×2.1 mm, 3.5 μm)	SB-C18 column (75 mm×2.1 mm, 3.5 μm)	SPE-UHPLC- MS/MS	0.65-0.67	2.21-2.23	82-88	4.8- 9.7	[46]
36 antibiotics	chicken meat	TurboFlow Cyclone- P (50 mm×0.5 mm, 60 μm)	Betasil phenyl hexyl column (50 mm×2.1 mm, 3 μm)	TFC-HPLC- MS/MS	300-40000	1000-120000	80-120	3-28	[47]
Ractopamine	beef	TurboFlow Cyclone- P (50 mm×0.5 mm, 60 μm)	Accucore C18 column (50 mm×3 mm, 2.6 μm)	TFC-HPLC- MS/MS	-	0.3	85-104	2.6- 14.0	[48]
5 benzimidazoles and 7 metabolites	milk	ADS column (25 mm ×4 mm, 25 μm)	Zorbax Eclipse XDB- C18 column (150 mm ×4.60 mm, 3 μm)	SPE-UHPLC- MS/MS	0.1-0.8	-	88-114	0.8- 9.7	[49]
8 quinolone antibacterials	milk, egg, chicken and fish	PEEK tube (poly (MAA-co-EGDMA), 150 mm×0.50 mm)	C18 column (250 mm ×2.0 mm, 5 μm)	In-tube SPME- LC/ESI-Q- TOF-MS	0.3-1.2 (egg), 0.2-3.0 (milk), 0.2-0.7 (chick- en), 0.2-1.0 (fish)	1.0-4.0 (egg), 0.6-10 (milk), 0.8-2.4 (chick- en), 0.6-3.3 (fish)	80.2- 115.0	1.3- 14.5	[50]

Analytes	Matrices	First dimension	Second dimension	On-line analysis system	LODs	LOQs	Recov- eries/%	RSDs/ %	Ref.
48 pesticide residues	wine	PS-DVB column (12.5 mm×2.1 mm, 15-20 μm)	Zorbax Eclipse XDB- C18 column (100 mm ×2.1 mm, 3.5 μm)	SPE-HPLC- MS/MS	-	0.02-2.5 μg/L	70-119	-	[52]
212 pesticides	fruits and vegetables	TurboFlow Cyclone-P (50 mm×0.5 mm, 60 μm)	Accucore aQ C18 col- umn (150 mm×2.1 mm, 2. 6 μm)	TFC-LC/ESI- Q-Orbitrap	-	0.5-5 μg/kg	58.3- 129.4	2.8- 16.0	[53]
15 amide herbicides	rice	poly(BMA-co-ED- MA) column (50 mm× 2.1 mm)	Hypersil GOLD col- umn (150 mm×2.1 mm, 5 μm)	TFC-HPLC- MS/MS	0.20-2.0 μg/kg	0.50-5.0 μg/kg	75.5- 121.3	2.89- 12.38	[54]
107 pesticides and metabolites	raw and drinking water	XBridge C18 column (30 mm×2.1 mm, 10 μm)	ACQUITY UHPLC HSS T3 column (100 mm× 2.1 mm, 1.8 μm)	SPE-UHPLC- MS/MS	0.03-1.5 ng/L	0.1-5.0 ng/L	61.2- 119.8	0.3-18.6	[55]
15 pesticide residues	cabbage and cucumber	XL C18 (50 mm×0.5 mm, silica type)	Phenomenex C18 col- umn (100 mm×2.1 mm, 1.7 μm)	TFC-HPLC- MS/MS	0.2-1.0 μg/kg	0.5-2.0 μg/kg	75.3- 103.7	0.3- 9.5	[16]
8 carbamate pesticide residues	tomato, rice, and cabbage	CAPCELL PAK C18 column (50 mm×2 mm, 15 μm)	ACQUITY UHPLC CSH C18 column (100 mm×2.1 mm, 1.7 μm)	SPE-HPLC- MS/MS	0.01-0.3 ng/mL	0.05-1.0 ng/mL	73.76- 112.32	1.28- 13.14	[56]

Analytes	Matrices	First dimension	Second dimension	On-line analysis system	LODs	LOQs	Recov- eries/%	RSDs/ %	Ref.
48 pesticide residues	wine	PS-DVB column (12.5 mm×2.1 mm, 15-20 μm)	Zorbax Eclipse XDB- C18 column (100 mm ×2.1 mm, 3.5 μm)	SPE-HPLC- MS/MS	-	0.02-2.5 μg/L	70-119	-	[52]
212 pesticides	fruits and vegetables	TurboFlow Cyclone-P (50 mm×0.5 mm, 60 μm)	Accucore aQ C18 col- umn (150 mm×2.1 mm, 2. 6 μm)	TFC-LC/ESI- Q-Orbitrap	-	0.5-5 μg/kg	58.3- 129.4	2.8- 16.0	[53]
15 amide herbicides	rice	poly(BMA-co-ED- MA) column (50 mm× 2.1 mm)	Hypersil GOLD col- umn (150 mm×2.1 mm, 5 μm)	TFC-HPLC- MS/MS	0.20-2.0 μg/kg	0.50-5.0 μg/kg	75.5- 121.3	2.89- 12.38	[54]
107 pesticides and metabolites	raw and drinking water	XBridge C18 column (30 mm×2.1 mm, 10 μm)	ACQUITY UHPLC HSS T3 column (100 mm× 2.1 mm, 1.8 μm)	SPE-UHPLC- MS/MS	0.03-1.5 ng/L	0.1-5.0 ng/L	61.2- 119.8	0.3-18.6	[55]
15 pesticide residues	cabbage and cucumber	XL C18 (50 mm×0.5 mm, silica type)	Phenomenex C18 col- umn (100 mm×2.1 mm, 1.7 μm)	TFC-HPLC- MS/MS	0.2-1.0 μg/kg	0.5-2.0 μg/kg	75.3- 103.7	0.3- 9.5	[16]
8 carbamate pesticide residues	tomato, rice, and cabbage	CAPCELL PAK C18 column (50 mm×2 mm, 15 μm)	ACQUITY UHPLC CSH C18 column (100 mm×2.1 mm, 1.7 μm)	SPE-HPLC- MS/MS	0.01-0.3 ng/mL	0.05-1.0 ng/mL	73.76- 112.32	1.28- 13.14	[56]

Analytes	Matrices	First dimension	Second dimension	On-line analysis system	LODs	LOQs	Recov- eries/%	RSDs/ %	Ref.
8 microcystins	fish	XBridge C18 Direct Connect HP column (30 mm×2.1 mm, 10 μm)	Waters Cortecs C18 column (100 mm×2.1 mm, 2.7 μm)	SPE-UHPLC- MS/MS	0.1-0.5 μg/kg	0.3-1.5 μg/kg	70.5- 98.9	1.3- 3.5	[58]
Ochratoxin A	red and white wine	Oasis MAX (20 mm× 2.1 mm, 12 μm)	Chromolith^® FastGra- dient column (50 mm ×2 mm)	SPE-UHPLC- MS/MS	0.012- 0.014 ng/mL	0.041- 0.045 ng/mL	80-88	3-6	[59]
Fumonisins	corn and wheat flour	WAX column (10 mm ×1 mm)	XBridge C18 column (150 mm×4.6 mm, 5 μm)	SPE-HPLC- MS/MS	0.08 μg/kg	0.2 μg/kg	93.9- 117.8	1.8- 9.4	[16]
Ochratoxin A	wine	PEEK tube (150 mm× 0.50 mm, C18)	XB-C18 (100 mm×2.1 mm, 2.6 μm)	In-tube SPME-HPLC- MS/MS	0.02 μg/L	0.05 μg/L	61.4- 72.8	1.15- 6.05	[60]
Aflatoxins (B1, B2, G1, and G2)	nuts, cereals, dried fruits, and spices	PEEK tube (60 cm× 0.32 mm, Supel- Q PLOT)	Zorbax Eclipse XDB- C8 column (150 mm× 4.6 mm, 5 μm)	In-tube SPME-UH- PLC-MS/MS	2.1-2.8 pg/mL	-	80.8- 109.1	1.9- 7.7	[61]
Aflatoxin M1	milk and dairy products	BioBasic C18 (20 mm ×2.0 mm, 5 μm)	Kinetex PFP column (100 mm×2.1 mm, 2.6 μm)	SPE-UHPLC-MS/MS	0.5-0.7 ng/kg	1.5-2.4 ng/kg	86-102	3-8	[62]
13 cyanotoxins	freshwater	ZIC-HILIC column (20 mm×2.1 mm, 5.0 μm)	Poroshell 120 HILIC-Z column (50 mm×2.1 mm, 1.9 μm)	SPE-HPLC- MS/MS	0.7-4.1 ng/L	1.8-8.1 ng/L	-	1.65- 13.02	[63]
Patulin	fruit juice and dried fruit	PEEK tube (60 cm× 0.32 mm, carbox- en 1006 PLOT)	Synergi MAX-RP 80A column (150 mm×4.6 mm, 4 μm)	In-tube SPME-UH- PLC-MS/MS	23.5 pg/mL		92.5- 94.4	0.95- 4.5	[64]

在线样品制备技术耦合液相色谱-质谱系统在食品危害物检测中的应用进展

Application progress of on-line sample preparation techniques coupled with liquid chromatography-mass spectrometry system in the detection of food hazards

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