水产品中有害物质分析样品前处理技术研究进展

doi:10.3724/SP.J.1123.2020.07025

色谱 ›› 2021, Vol. 39 ›› Issue (1): 34-45.DOI: 10.3724/SP.J.1123.2020.07025

水产品中有害物质分析样品前处理技术研究进展

王兴益¹^,², 陈彦龙¹, 肖小华¹^,^*(), 李攻科¹^,^*()

1.中山大学化学学院, 广东广州 510275
2.兴义民族师范学院生物与化学学院, 贵州兴义 562400

收稿日期:2020-08-13 出版日期:2021-01-08 发布日期:2020-12-20
通讯作者: 肖小华,李攻科
作者简介:Tel:(020)84110922,E-mail:cesgkl@mail.sysu.edu.cn(李攻科).

肖小华: 博士,中山大学化学学院副教授,博士生导师。本科毕业于湘潭大学,2005年7月在中科院兰州化物所获博士学位,2014年到美国俄克拉荷马大学交流访学。主要从事复杂样品分离分析及样品前处理技术、装置研制等研究工作。主持国家自然科学基金(4项)、广东省自然科学基金(3项)等科研项目共10余项。并作为骨干参加国家重大仪器研究专项、国家自然科学基金仪器专项、广东省自然科学基金重点项目等科研项目10余项。在Anal Chem, J Chromatogr A等国内外期刊发表论文60余篇,申请中国发明专利8件(其中授权专利3件)。获2017年度教育部自然科学成果二等奖1项及广东省科技成果三等奖1项(排名第三)。现任J Sep Sci编委,以及Chin Chem Lett和《色谱》青年编委,为中国产学研合作促进会中国生物检测监测产业技术创新战略联盟理事、中国仪器仪表学会分析仪器分会青年工作委员会/关键部件委员会委员、广东省分析测试协会色谱专业委员会秘书。*Tel:(020)84110922,E-mail:xiaoxhua@mail.sysu.edu.cn(肖小华);
基金资助:
广东省重点领域研发计划食品安全重点专项(2019B020211001);国家重点研发计划课题(2019YFC1606101);国家自然科学基金项目(21976213);国家自然科学基金项目(21675178);国家自然科学基金项目(21675179)

Recent advances in sample preparation technologies for analysis of harmful substances in aquatic products

WANG Xingyi¹^,², CHEN Yanlong¹, XIAO Xiaohua¹^,^*(), LI Gongke¹^,^*()

1. School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China
2. School of Biology and Chemistry, Xingyi Normal University for Nationalities, Xingyi 562400, China

Received:2020-08-13 Online:2021-01-08 Published:2020-12-20
Contact: XIAO Xiaohua,LI Gongke
Supported by:
Research and Development Plan for Key Areas of Food Safety in Guangdong Province of China(2019B020211001);National Key Research and Development Program of China(2019YFC1606101);National Natural Science Foundation of China(21976213);National Natural Science Foundation of China(21675178);National Natural Science Foundation of China(21675179)

摘要/Abstract

摘要：

水产品含有丰富的蛋白、维生素和多种微量元素,是人们摄取动物性蛋白质的重要来源之一,我国是世界上最大的水产品消费国,其质量安全问题一直备受关注。但水产样品基质复杂,有害物质的含量低,须对其进行分离富集后才能进行检测,传统的液-液萃取、固相萃取和快速固相分散萃取等样品前处理技术在水产品分析中得到广泛应用,同时针对一些挥发性和超痕量有害物质检测时,固相微萃取同样体现出巨大优势。这些样品前处理技术可以有效去除基体对分析对象的干扰,提高检测方法的灵敏度和准确度。根据目标分析物性质的不同,选择合适的样品前处理技术,是水产品中有害物质分析的关键步骤。该文以水产品中有害物的来源不同,将其分为3类:(1)水产品中环境污染物的分析;(2)养殖运输和加工过程中有害物的分析;(3)水产品中生物毒素的分析。以这3类有害物质的分析为主线,综述了近10年水产品中有害物质分析的样品前处理技术,包括液-液萃取、固相萃取、固相微萃取、快速固相分散萃取和磁性固相萃取等。此外,还对各种技术的优缺点进行了探讨,并对其未来发展方向进行了展望。

关键词: 样品前处理, 环境污染物, 非法添加剂, 生物毒素, 水产品

Abstract:

Aquatic products, which are among the most important sources of animal protein, contain proteins, vitamins, and a variety of trace elements, thus occupying an indispensable part of a reasonable diet. China is the largest consumer market of aquatic products in the world. The quality and safety of aquatic products are closely related not only to the healthy development of the aquaculture industry, but also to people’s health. However, the presence of harmful substances has a bearing on the quality and safety of aquatic products in the overall process, including breeding, processing, storage, and transportation. These harmful substances are enriched in aquatic products and are transferred to humans via the food chain. Accurate determination of such harmful substances in aquatic product samples is imperative because of their complex matrices and extremely low concentrations. Many efficient sample preparation techniques such as liquid-liquid extraction, solid-phase extraction, and QuEChERS (quick, easy, cheap, effective, rugged, and safe method) with different configurations have been developed and widely employed for preconcentration in different matrices of aquatic products. Meanwhile, solid-phase microextraction has been demonstrated to be advantageous for some volatile and ultra-trace harmful substances. Suitable sample preparation techniques are important for effectively removing matrix interferences as well as for improving the sensitivity and accuracy of the method. It is important to develop appropriate sample preparation techniques for different target compounds in aquatic products. The harmful substances in aquatic products can be segregated into three categories according to their sources: (1) environmental pollutants in aquatic products; (2) substances acquired during aquaculture, transportation, and processing; (3) biotoxins in aquatic products. This article reviews the progress in sample pretreatment techniques for three harmful substances in aquatic products over the past decade. Various sample pretreatment techniques have been summarized and described, including liquid-liquid extraction, solid-phase extraction, solid-phase microextraction, QuEChERS, and magnetic solid-phase extraction. In addition, the merits and demerits of these techniques and future research directions are discussed. Finally, we reviewed the progress in functionalized materials for the preparation of aquatic product samples. With the increasing demand for aquatic products, quick, sensitive, and practical detection methods, such as surface-enhanced Raman scattering (SERS) are gaining importance. SERS has great potential for fast and accurate on-site detection of harmful substances in aquatic products. Several nondestructive sample pretreatment techniques have also been developed for harmful substances in aquatic products. The application and development of these techniques will guarantee the safety of aquatic products. Moreover, in vivo solid-phase microextraction is a potential method for aquatic product analysis. This technique integrates sampling, extraction, and enrichment into a single step, thus significantly reducing the processing time, labor, and cost. Overall, with the development and application of sophisticated materials and techniques, we can expect theoretical and practical advances in aquatic product analysis.

Key words: sample preparation, environmental pollutants, illegal additive, biotoxins, aquatic products

中图分类号:

O658

王兴益, 陈彦龙, 肖小华, 李攻科. 水产品中有害物质分析样品前处理技术研究进展[J]. 色谱, 2021, 39(1): 34-45.

WANG Xingyi, CHEN Yanlong, XIAO Xiaohua, LI Gongke. Recent advances in sample preparation technologies for analysis of harmful substances in aquatic products[J]. Chinese Journal of Chromatography, 2021, 39(1): 34-45.

图/表 7

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Preparation technology	Sample	Analyte	Analytical method	LOD		Ref.
LLE	shrimp	PCBs	GC-MS	0.02-0.14	μg/L	[28]
ASE	fish	PCBs	GC-MS	0.1-0.5	ng/kg	[29]
SPME	fish, shrimp	PCBs	GC-MS	0.07-0.35	ng/L	[30]
MSPE	fish	PCBs	GC-MS	0.061-0.096	ng/g	[31]
ULLE	fish	PAHs	GC-MS	0.12-0.25	μg/kg	[32]
QuEChERS	shrimp, crab	PAHs	HPLC-FLD	0.2-2.0	μg/kg	[33]
SPE	shellfish	PAHs	HPLC-VWD/FLD	0.5	μg/kg	[34]
SPME	fish	PAHs	GC-MS	0.11-1.40	μg/kg	[35]
LLE	fish, shrimp	chlorinated phenols	GC-MS	0.78	μg/kg	[37]
SPE	shrimp, crab	pentachlorophenol	HPLC-MS	0.2	μg/kg	[38]
MSPE	shrimp	phenolic endocrine	HPLC-FLD	1.4-8.7	μg/L	[39]
QuEChERS	fish, shellfish	PFASs	LC-MS/MS	0.006-0.02	μg/kg	[40]
SPE	fish	PFASs	UPLC-MS/MS	2-120	pg/g	[41]
LLE	shellfish	Pesticide	GC-MS/MS	0.7-3.3	μg/kg	[42]
MIP-SPE	fish	pyrethroid insecticide	GC-ECD	16.1-26.5	ng/kg	[43]
SPME	fish	sulfonamides	UPLC-MS/MS	1.3-4.7	ng/L	[44]
MSPE	shrimp	sulfonamides	UPLC-VWD	0.2-1	ng/mL	[45]
LLE	fish	Hg	HPLC-ICP-MS	0.09-0.18	ng/mL	[46]
DLLME-SFO	fish	Cd, Pb	GFAAS	0.04-0.1	μg/kg	[47]
SPE	fish	Pb, Cu	ICP-OES	1.434, 0.048	μg/L	[48]
IIPs-SPE	fish	Cd, Pb	ETAAS	0.15, 0.5	μg/L	[49]
MSPE	fish	Ag, Cd, Pb, Hg, Cu	ICP-OES	0.01-0.09	ng/mL	[50]
MR/IT-SPME	fish	Cu, Co, Hg	HPLC-DAD	0.69-4.9	μg/kg	[51]

Preparation technology	Sample	Analyte	Analytical method	LOD		Ref.
LLE	shrimp	PCBs	GC-MS	0.02-0.14	μg/L	[28]
ASE	fish	PCBs	GC-MS	0.1-0.5	ng/kg	[29]
SPME	fish, shrimp	PCBs	GC-MS	0.07-0.35	ng/L	[30]
MSPE	fish	PCBs	GC-MS	0.061-0.096	ng/g	[31]
ULLE	fish	PAHs	GC-MS	0.12-0.25	μg/kg	[32]
QuEChERS	shrimp, crab	PAHs	HPLC-FLD	0.2-2.0	μg/kg	[33]
SPE	shellfish	PAHs	HPLC-VWD/FLD	0.5	μg/kg	[34]
SPME	fish	PAHs	GC-MS	0.11-1.40	μg/kg	[35]
LLE	fish, shrimp	chlorinated phenols	GC-MS	0.78	μg/kg	[37]
SPE	shrimp, crab	pentachlorophenol	HPLC-MS	0.2	μg/kg	[38]
MSPE	shrimp	phenolic endocrine	HPLC-FLD	1.4-8.7	μg/L	[39]
QuEChERS	fish, shellfish	PFASs	LC-MS/MS	0.006-0.02	μg/kg	[40]
SPE	fish	PFASs	UPLC-MS/MS	2-120	pg/g	[41]
LLE	shellfish	Pesticide	GC-MS/MS	0.7-3.3	μg/kg	[42]
MIP-SPE	fish	pyrethroid insecticide	GC-ECD	16.1-26.5	ng/kg	[43]
SPME	fish	sulfonamides	UPLC-MS/MS	1.3-4.7	ng/L	[44]
MSPE	shrimp	sulfonamides	UPLC-VWD	0.2-1	ng/mL	[45]
LLE	fish	Hg	HPLC-ICP-MS	0.09-0.18	ng/mL	[46]
DLLME-SFO	fish	Cd, Pb	GFAAS	0.04-0.1	μg/kg	[47]
SPE	fish	Pb, Cu	ICP-OES	1.434, 0.048	μg/L	[48]
IIPs-SPE	fish	Cd, Pb	ETAAS	0.15, 0.5	μg/L	[49]
MSPE	fish	Ag, Cd, Pb, Hg, Cu	ICP-OES	0.01-0.09	ng/mL	[50]
MR/IT-SPME	fish	Cu, Co, Hg	HPLC-DAD	0.69-4.9	μg/kg	[51]

Preparation technology	Sample	Analyte	Analytical method	LOD		Ref.
MAE-LLE	fish	steroid hormones	LC-MS	0.03-0.15	ng/g	[52]
QuEChERS	fish, shrimp	hormones	UPLC-MS	0.2-2.7	μg/kg	[53]
MAE-SPE	fish	steroid hormones	UPLC-MS/MS	0.14-49.0	ng/g	[54]
MIP-SPE	fish, shrimp	estrogens	HPLC-FLD	0.023	mg/L	[55]
LLE	shrimp	nitrofuran	HPLC-FLD	0.24-0.26	μg/kg	[56]
IL-DLLME	fish	fluoroquinolones	HPLC-DAD	0.5-1.1	ng/mL	[57]
QuEChERS	fish, shrimp	chlorpyrifos	HPLC-MS/MS	0.25	μg/kg	[58]
SPE	fish	florfenicol amine	LC-MS/MS	0.13-1.64	μg/kg	[59]
MIP-MSPE	fish, shrimp	macrolide	HPLC-UV	0.015-0.2	μg/g	[60]
MSPE	fish	nitrofurantoin	SERS	0.014	mg/L	[61]
SPME	fish	fluoroquinolones	LC-MS	0.3-1.5	ng/g	[62]
DLLME	fish	menthol	GC-MS	0.0539	μg/L	[63]
QuEChERS	fish	tricaine mesylate	HPLC-MS/MS	2.5	μg/kg	[64]
SPE	fish, shrimp	diazepam	UPLC-MS	0.5	μg/kg	[65]
SPE	fish, shrimp	eugenol	UPLC-MS	0.3-0.75	μg/kg	[66]
SPME	fish	anesthetics	GC-MS	1.7-9.4	ng/g	[67]
SPME	fish	2-phenoxyethanol	HPLC-MS	0.18	μg/mL	[68]
LLE	fish	4-hexylresorcinol	UPLC-FLD	2.0	mg/kg	[69]
LLE	squid	formaldehyde	GC-MS	2.0	mg/kg	[70]
SPME	fish	formaldehyde	GC-MS	17	μg/kg	[71]
HS-SPME	fish	trihalomethanes	GC-MS	0.11-0.35	μg/kg	[72]

Preparation technology	Sample	Analyte	Analytical method	LOD		Ref.
MAE-LLE	fish	steroid hormones	LC-MS	0.03-0.15	ng/g	[52]
QuEChERS	fish, shrimp	hormones	UPLC-MS	0.2-2.7	μg/kg	[53]
MAE-SPE	fish	steroid hormones	UPLC-MS/MS	0.14-49.0	ng/g	[54]
MIP-SPE	fish, shrimp	estrogens	HPLC-FLD	0.023	mg/L	[55]
LLE	shrimp	nitrofuran	HPLC-FLD	0.24-0.26	μg/kg	[56]
IL-DLLME	fish	fluoroquinolones	HPLC-DAD	0.5-1.1	ng/mL	[57]
QuEChERS	fish, shrimp	chlorpyrifos	HPLC-MS/MS	0.25	μg/kg	[58]
SPE	fish	florfenicol amine	LC-MS/MS	0.13-1.64	μg/kg	[59]
MIP-MSPE	fish, shrimp	macrolide	HPLC-UV	0.015-0.2	μg/g	[60]
MSPE	fish	nitrofurantoin	SERS	0.014	mg/L	[61]
SPME	fish	fluoroquinolones	LC-MS	0.3-1.5	ng/g	[62]
DLLME	fish	menthol	GC-MS	0.0539	μg/L	[63]
QuEChERS	fish	tricaine mesylate	HPLC-MS/MS	2.5	μg/kg	[64]
SPE	fish, shrimp	diazepam	UPLC-MS	0.5	μg/kg	[65]
SPE	fish, shrimp	eugenol	UPLC-MS	0.3-0.75	μg/kg	[66]
SPME	fish	anesthetics	GC-MS	1.7-9.4	ng/g	[67]
SPME	fish	2-phenoxyethanol	HPLC-MS	0.18	μg/mL	[68]
LLE	fish	4-hexylresorcinol	UPLC-FLD	2.0	mg/kg	[69]
LLE	squid	formaldehyde	GC-MS	2.0	mg/kg	[70]
SPME	fish	formaldehyde	GC-MS	17	μg/kg	[71]
HS-SPME	fish	trihalomethanes	GC-MS	0.11-0.35	μg/kg	[72]

Preparation technology	Sample	Analyte	Analytical method	LOD		Ref.
SPE	shellfish	yessotoxin	LC-MS/MS	0.15-0.30	μg/kg	[77]
SPE	shellfish	shellfish toxin	LC-MS/MS	0.1-1.1	μg/kg	[79]
QuEChERS	shellfish	shellfish toxin	UPLC-MS/MS	0.3	μg/kg	[80]
QuEChERS	shellfish	marine toxin	UPLC-MS/MS	0.10-1.47	μg/kg	[81]
MSPE	shellfish	domoic acid	HPLC-MS/MS	1.45	pg/mL	[82]
MSPE	shellfish	domoic acid	HPLC-MS/MS	0.2	pg/mL	[83]
SPME	fish	biogenic amines	GC-MS	2.98-45.3	μg/kg	[84]
SPE	pufferfish	tetrodotoxin	LC-MS/MS	2.3	ng/g	[86]

水产品中有害物质分析样品前处理技术研究进展

Recent advances in sample preparation technologies for analysis of harmful substances in aquatic products

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