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Chinese Journal of Chromatography
2020, Vol. 38, No. 1
Online: 08 January 2020

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Volume 38, Number 1 Content 2020, 38 (1):  0-0.  Abstract ( 24 )   PDF (5546KB) ( 27 )

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Preface for the Special Issue of Progress in Sample Preparation Technology in China 2020, 38 (1):  1-1.  DOI: 10.3724/SP.J.1123.2019.10033 Abstract ( 38 )   HTML ( 172 )   PDF (527KB) ( 41 )

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Progress in application of functionalized magnetic nanomaterials for sample pretreatment LI Fei, WU Haocheng, LI Yijun, HE Xiwen, CHEN Langxing, ZHANG Yukui 2020, 38 (1):  2-13.  DOI: 10.3724/SP.J.1123.2019.06034 Abstract ( 118 )   HTML ( 172 )   PDF (1237KB) ( 110 )   With the increasing complexity of the sample properties in analytical chemistry and the lower concentrations of the detected substances, it is imperative to develop accurate and efficient sample pretreatment processes before chromatography and mass spectrometry analyses. Magnetic solid-phase extraction (MSPE) can be regarded as an efficient sample pretreatment method due to the simple synthesis, convenient operation, and high extraction efficiency. In recent years, Fe3O4 magnetic nanomaterials have been widely used in separation and analysis due to their advantages such as high separation speed, good dispersion, and biocompatibility. Functionalized Fe3O4 magnetic nanomaterials are expected to show greatly improved physical and chemical stability, with superior adsorption and separation ability. In this paper, the preparation of magnetic nanomaterials functionalized with carbon-based nanomaterials, molecularly imprinted polymers, ionic liquids, boronate affinity ligands, metal organic frameworks, covalent organic frames, quantum dots, and metal oxides and their applications to sample pretreatment in the fields of biological, environmental, and food safety are reviewed. In addition, future research on sample pretreatment processes is prospected.

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Advances in magnetic nanomaterials for sample pretreatment and future prospects DING Qingqing, ZHANG Wenmin, ZHANG Lan 2020, 38 (1):  14-21.  DOI: 10.3724/SP.J.1123.2019.07001 Abstract ( 103 )   HTML ( 162 )   PDF (1617KB) ( 91 )   Adsorbent materials play a key role in sample preparation techniques. With the recent developments in this field, increasing numbers of nanomaterials are being used as adsorbents to improve the extraction efficiency of the target compound. Because of their advantages such as ease of separation, facile surface modification, strong adsorption capacity, and good biocompatibility, magnetic nanomaterials have been widely used for sample preparation techniques in analytical chemistry. In this paper, research trends in magnetic nanomaterials and their application to magnetic solid-phase extraction and other sample pretreatment techniques are summarized and discussed. The stability, force, specific surface area, and pore size control of the magnetic nanomaterials are also described. The application prospects of magnetic nanomaterials in separation science are prospected, which provides a clear outlook and reference for further research into their application.

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Recent advances in the application of metal-organic frameworks for sample pretreatment QIAN Hailong, YAN Xiuping 2020, 38 (1):  22-27.  DOI: 10.3724/SP.J.1123.2019.07017 Abstract ( 104 )   HTML ( 161 )   PDF (831KB) ( 72 )   Metal-organic frameworks (MOFs) have been widely applied in the fields of energy storage, catalysis, sensing, and separation. Their diverse structural topologies, large surface areas, and tunable pore sizes, also make MOFs great application potential in sample pretreatment. New sample pretreatment methods using MOFs are continually being developed. This review summaries the state-of-the art for the application of the powders, films, nanosheets and composites of MOFs in sample pretreatment, including solid phase extraction, solid phase microextraction, and magnetic solid phase extraction. Future prospects of MOFs in sample pretreatment are also presented.

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Recent advances in graphitic carbon nitride materials for sample pretreatment HAN Lizhen, YANG Yixin, ZHANG Jing, GUO Jinggong, LU Minghua 2020, 38 (1):  28-35.  DOI: 10.3724/SP.J.1123.2019.06032 Abstract ( 138 )   HTML ( 169 )   PDF (2084KB) ( 74 )   As a new type of non-metallic material, graphite carbon nitride (g-C3N4) has attracted increasing attention due to its inherent advantages such as simple preparation, excellent thermal and chemical stability, as well as good biocompatibility and non-toxicity. Nowadays, g-C3N4 is widely used in electrocatalysis, photocatalysis, biological imaging, and so on. Because of its large specific surface area, π -electron-rich structure, and hydrophobic properties, g-C3N4 is considered an ideal candidate material for sample pretreatment. In this work, g-C3N4 and its composites as potential sorbents for solid-phase extraction, dispersive solid-phase extraction, magnetic solid-phase extraction, and solid-phase microextraction are reviewed, and the future trends and prospective are discussed.

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Application of carbon dots in sample pretreatment and chromatographic separation YUAN Ning, CHEN Jia, GUAN Ming, ZHAO Liang, QIU Hongdeng 2020, 38 (1):  36-40.  DOI: 10.3724/SP.J.1123.2019.06001 Abstract ( 83 )   HTML ( 167 )   PDF (2061KB) ( 57 )   Carbon dots (CDs) have the advantages of good biocompatibility, low toxicity and high stability, and have been widely used in bioimaging, sensing, photocatalysis, etc. In recent years, sample pretreatment and chromatographic separation studies using CDs as adsorbents and separation materials have also attracted much interest. In this review, the applications of CDs in sample pretreatment and chromatographic separation are summarized, and further development prospects are prospected.

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Recent advances in the application of thin-film microextraction GUO Zhiyong, YAO Qiuhong, LIN Qi, CHEN Xi 2020, 38 (1):  41-49.  DOI: 10.3724/SP.J.1123.2019.05008 Abstract ( 142 )   HTML ( 165 )   PDF (1080KB) ( 70 )   Thin-film microextraction (TFME), which is a new technique in solid-phase microextraction and correlational research, have gradually attracted the attention of scientists in the field of sample preparation. Because of the high surface area-to-volume ratio and the concurrent increase inthe extraction-phase volume, TFME shows enhanced sensitivity without sacrificing the sampling time, as opposed to other microextraction approaches. Recently, TFME in combination with sample analysis techniques has been widely used for the analysis of forbidden drugs, explosives, pesticides, and veterinary drugs in the pharmaceutical, foodstuff, and environmental industries. This review summarizes the fundamentals, formats, and applications of TFME, as well as its long-term prospects and potential applications.

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Recent advances in molecular imprinting technology for the separation and analysis of proteins SUN Xiaoyu, MA Runtian, SHI Yanping 2020, 38 (1):  50-59.  DOI: 10.3724/SP.J.1123.2019.06017 Abstract ( 133 )   HTML ( 175 )   PDF (2931KB) ( 92 )   Proteins, which have complex structures and fall under diverse categories, are closely associated with different kinds of life activities. Majority of the proteins exist in low concentrations in complex biological samples, because of which their direct analysis without sample pretreatment is difficult. Thus, selective separation of the target proteins from complex biological samples is essential for efficient analysis. Molecularly imprinted polymers, containing numerous imprinted cavities that are complementary with the templates in terms of shape, size, and functional groups, have great potential for use in the selective recognition and separation of the target proteins from complex biological samples. However, the large size, structural flexibility, and complex structures of proteins hinder their efficient separation and analysis by conventional molecular imprinting technology. In this review, several novel molecular imprinting techniques, including surface imprinting, epitope imprinting, and metal chelate imprinting, are introduced. The emergence of these novel technologies has contributed to advances in protein analysis. The applications of these molecular imprinting techniques to the separation and analysis of proteins in the last three years are summarized herein. Finally, the promising future of molecular imprinting techniques in the area of proteins is prospected.

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Application of functionalized magnetic nanomaterials in phosphopeptide enrichment XIONG Fangfang, JIANG Dandan, JIA Qiong 2020, 38 (1):  60-65.  DOI: 10.3724/SP.J.1123.2019.06019 Abstract ( 69 )   HTML ( 165 )   PDF (821KB) ( 51 )   Protein phosphorylation is one of the most important and prevalent post-translational modifications. Mass spectrometry (MS) has become a powerful tool for the analysis of phosphopeptides. However, the low dynamic stoichiometry, poor ionization efficiency, and signal suppression by high-abundance non-phosphorylated peptides have hindered the direct applications in the analysis of phosphopeptides. Therefore, the development of highly selective and sensitive enrichment strategies is necessary for the identification of phosphopeptides prior to MS analysis. Magnetic nanomaterials have good magnetic responsiveness and can be separated rapidly from the solution with the help of external magnets. Functionalized magnetic nanomaterials have been widely used as a new analytical tool in proteomics research. This review surveys recently reported functionalized magnetic nanoparticles for the enrichment of phosphopeptides reported in recent years. Further trends in the enrichment of phosphopeptides with functionalized magnetic materials are also prospected.

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Advances in the development of the sample preparation techniques in lipidomics SONG Shiyao, BAI Yu, LIU Huwei 2020, 38 (1):  66-73.  DOI: 10.3724/SP.J.1123.2019.07011 Abstract ( 260 )   HTML ( 173 )   PDF (2201KB) ( 133 )   Lipids play an important physiological role in living system. They are the major components of cellular membranes, in addition to participating in energy storage as well as signal recognition and transmission. In recent years, an increasing number of studies have shown that disturbances in lipid metabolism are closely related to the development of some diseases. Lipid analysis is of great significance for understanding the mechanism and the process of diseases. Because of the matrix interference and low concentration of analytes, existing techniques require sample preparation steps to ensure good analytical performance. In the present study, sample preparation methods in lipidomics used in various fields are reviewed, including lipid extraction methods, such as liquid-liquid extraction and solid phase extraction, as well as the chemical derivatization techniques for different lipid categories. In addition, the development of the sample preparation in lipidomics is also prospected.

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Recent advances in sample preparation techniques for the lipid profiling based on chromatography-mass spectrometry YANG Jina, LIU Danyang, ZHOU Ting 2020, 38 (1):  74-85.  DOI: 10.3724/SP.J.1123.2019.06023 Abstract ( 134 )   HTML ( 161 )   PDF (983KB) ( 71 )   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.

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Progress on the sample techniques and analytical methods for typical perfluorinated organic acids HE Jincan, ZHANG Shiyun, SU Yuyuan, SONG Jiayi, WU Fuhai 2020, 38 (1):  86-94.  DOI: 10.3724/SP.J.1123.2019.06016 Abstract ( 254 )   HTML ( 192 )   PDF (898KB) ( 131 )   Perfluorooctanesulfonate (PFOS) and perfluorooctanoic acid (PFOA) are typical perfluorinated organic acids with hepatotoxicity, embryonic toxicity, reproductive toxicity, and neurotoxicity. As the final degradation products of perfluorochemicals (PFCs) precursors, PFOS and PFOA are detected frequently. Presently, there are no unified standards for the detection of PFOS and PFOA. The analytical techniques used for PFCs in China are much less sophisticated than those in the developed countries. In this paper, the characteristics of PFOS and PFOA are introduced. Sample preparation technologies (liquid-liquid extraction, solid-phase extraction, solid-phase microextraction, ultrasonic extraction, and QuEChERS), and analytical methods (chromatography-mass spectrometry, spectrometry, ELISA, and electrochemical methods) are summarized and reviewed, so as to provide reference for monitoring and setting standards.

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Advances in sample pretreatment techniques for analysis of antibiotics in the coastal environment LÜ Min, CHEN Lingxin 2020, 38 (1):  95-103.  DOI: 10.3724/SP.J.1123.2019.07005 Abstract ( 85 )   HTML ( 172 )   PDF (2787KB) ( 54 )   The widespread and massive usage of antibiotics for the prevention and treatment of diseases in human and animals have resulted in their continuous discharge into the environment, and finally, into the coastal environment through various pathways. Accumulation of antibiotics in aquatic organisms poses a great threat to ecological and human health, especially because it facilitates the generation and spread of bacterial resistance. Given the diverse range of antibiotics with various features, as well as their presence at low concentrations in the environment, it is imperative to develop pretreatment techniques for antibiotics in various matrices. In this paper, the pretreatment methods proposed in recent decades for antibiotics in coastal water, sediment, and biota are summarized, with emphasis on commonly used methods such as solid-phase extraction, solid-liquid extraction, matrix solid-phase dispersion, and QuEChERS. Additionally, the potential factors influencing the extraction performance and clean-up efficiency are analyzed. The advantages and disadvantages of the methods and their development are finally discussed.

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Progress in application of molecularly imprinted polymers based on β-cyclodextrin to environmental and food sample pretreatment HE Zhongyu, CUI Yahan, HUANG Ning, YANG Shuliang, CHEN Yanhua, DING Lan 2020, 38 (1):  104-112.  DOI: 10.3724/SP.J.1123.2019.06013 Abstract ( 67 )   HTML ( 162 )   PDF (3102KB) ( 57 )   β-cyclodextrin (β-CD) and its derivatives are an emerging class of functional monomers that find widespread use in molecular imprinting. It is well known that β-CD and its derivatives are capable of forming host-guest interaction inclusion complexes with many guest molecules. Molecularly imprinted polymers prepared via this type of interaction have the advantages of high stability and excellent selectivity. Therefore, β-CD-based molecularly imprinted polymers have attracted much attention and have been extensively developed for the selective separation and enrichment of target compounds in environmental and food samples with complex matrices. The objective of this review is to reveal the advantages of such molecularly imprinted polymers in complex sample pretreatment by reviewing the applications of molecularly imprinted polymers based on β-CD and its derivatives as functional monomers in environmental and food sample pretreatment since 2013.

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Determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry based on magnetic conjugated microporous polymers CAI Weiqiu, LEI Haoyu, HU Yuling, LI Gongke 2020, 38 (1):  113-119.  DOI: 10.3724/SP.J.1123.2019.06033 Abstract ( 85 )   HTML ( 170 )   PDF (1582KB) ( 71 )   A method was developed for the determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on magnetic conjugated microporous polymers (CMPs). Fe3O4 nanoparticles modified by phenylene and ethynylene were cross-linked with 1, 3, 5-tribromobenzene and 1, 3, 5-trialkynylbenzene to obtain magnetic CMPs. This material with a three-dimensional network structure and covalently built-in Fe3O4 nanoparticles could effectively enrich organophosphorus insecticides with a conjugated structure, thus allowing for convenient magnetic separation in an external magnetic field. Under the optimized conditions, the seven organophosphorus pesticides were extracted by using the magnetic CMPs as magnetic solid phase extraction adsorbents. The limits of detection (LODs) of the seven target analytes were in the range of 0.12-5.0 ng/kg. The recoveries were between 80.8% and 125%, and the relative standard deviations (RSDs, n=5) were less than 6%. The organophosphorus insecticides were detected in fruits and vegetables at concentrations in the range of 1.1-500.0 ng/kg. The method is sensitive, accurate and reliable, and it shows good application potential for the determination of the organophosphorus pesticides in fruits and vegetables.

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Rapid determination of 12 semi-volatile pesticide residues in vegetables by miniaturized thermal-assisted purge-and-trap coupled with ultra high pressure liquid chromatography-tandem mass spectrometry CHEN Zhengyi, LI Yunda, ZHANG Zhuomin, LI Gongke 2020, 38 (1):  120-126.  DOI: 10.3724/SP.J.1123.2019.01051 Abstract ( 72 )   HTML ( 168 )   PDF (2066KB) ( 53 )   A method for the analysis of 12 semi-volatile pesticide residues in vegetables was developed by miniaturized thermal-assisted purge-and-trap coupled with ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Under the optimized conditions, the sample preparation could be completed within 10 min. The linear relationships of the 12 semi-volatile pesticide residues were good within their corresponding concentration ranges. The correlation coefficients were in range of 0.9918-0.9997. The limits of detection and limits of quantification were in range of 0.3-1.3 μg/kg and 1.0-4.3 μg/kg, respectively. The recoveries ranged from 80.0% to 120.0%, with intra-day and inter-day RSDs of less than 10%. This proposed method is quick and simple, and is suitable for the simultaneous and rapid analysis of semi-volatile pesticide residues in vegetables.

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Analysis of four preservatives in beverages and instant noodle samples by high performance liquid chromatography-ultraviolet detection coupled with magnetic solid phase extraction based on metal-organic frameworks XIAO Zuowei, HE Man, CHEN Beibei, HU Bin 2020, 38 (1):  127-136.  DOI: 10.3724/SP.J.1123.2019.06014 Abstract ( 89 )   HTML ( 165 )   PDF (2223KB) ( 57 )   Magnetic amino functionalized metal-organic frameworks (MOFs) were prepared by a simple stirring and blending process. The obtained composites had good magnetic and thermal stability with a large specific surface area, and were used for the extraction of four preservatives with different polarities (benzoic acid, sorbic acid, propyl p-hydroxybenzoate and butyl p-hydroxybenzoate) in soda water, vitamin beverage and instant noodle cake samples. After optimizing the conditions for magnetic solid phase extraction (MSPE) and desorption, the four preservatives were analysed by a high performance liquid chromatography-ultraviolet detection (HPLC-UV) method. The analytes were separated on a Purospher® STAR LP C18 column (250 mm×4.6 mm, 5 μm). Methanol and 10 mmol/L ammonium acetate aqueous solution (50:50, v/v) were used as the mobile phases with gradient elution. The limits of detection of the four preservatives were 0.51-1.89 μg/L. The recoveries of the target preservatives were 72.2%-109% in the soda water, vitamin beverage and instant noodle cake samples. The method is simple, rapid, accurate and reliable, and is suitable for the analysis of preservatives with different polarities in beverages and foods. The method can provide an effective technology for food safety and quality control.

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Automated hyphenation of in-tube boronate affinity solid-phase microextraction with high performance liquid chromatography for the determination of cis-diol compounds in tea beverages WANG Xin, HE Jiangang, LUO Qi, LIU Zhen 2020, 38 (1):  137-142.  DOI: 10.3724/SP.J.1123.2019.06020 Abstract ( 72 )   HTML ( 164 )   PDF (2416KB) ( 44 )   Automatic hyphenated analytical techniques hold great promise for reducing labour intensity, enhancing efficiency, and ensuring data reproducibility. In recent decade, Boronate affinity solid phase microextraction (BA-SPME) has emerged as a unique tool for the selective extraction of cis-diol-containing compounds. However, automatic hyphenation of SPME with high performance liquid chromatography (HPLC) has not yet been reported. Herein we report a new automated hyphenation of in-tube BA-SPME with HPLC for the determination of cis-diol compounds in tea beverages. The automated hyphenation was implemented through a flow-switch via the six-way valve of an autosampler. We prepared an in-tube SPME capillary, investigated the loading capacity of the coated column, characterized the morphology of the column, and investigated the factors influencing the separation. Finally, using the automatic hyphenated SPME-HPLC approach, we analyzed the cis-diol-containing compounds in three kinds of commercial tea beverages and investigated the effect of tea-making temperature on the content of the cis-diol-containing compounds in the prepared tea.

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Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water PENG Zifang, LI Qin, ZHANG Guangrui, ZHAO Wuduo, LIAN Hongzhen, ZHANG Shusheng 2020, 38 (1):  143-148.  DOI: 10.3724/SP.J.1123.2019.06022 Abstract ( 52 )   HTML ( 164 )   PDF (1772KB) ( 22 )   A novel method based on solid phase extraction (SPE)-high performance liquid chromatography (HPLC) was developed for the simultaneous determination of nitrophenols and diethylstilbestrol in river water. Tetraaza[2]arene[2]triazine-bonded silica gel, a homemade SPE adsorbent, was used to enrich the nitrophenols and diethylstilbestrol, and the optimal SPE and HPLC conditions were established. The sample solution was adjusted to pH 5, purified with a lab-made solid phase extraction column, and then eluted with 2 mL ammonia-methanol (2:98, v/v). The enriched sample was separated on a C8 column with methanol and 0.1% phosphoric acid solution as mobile phases in a gradient elution. Under the optimized conditions, the limits of detection (LOD, S/N=3) for the four target analytes were 0.03-0.3 μg/L, and the limits of quantification (LOQ, S/N=10) were 0.1-1.0 μg/L. The recoveries were 75.5%-104.2%, and the relative standard deviations (RSD, n=5) were less than 6.3%. The proposed method is accurate and reliable, and it has been successfully used for determining nitrophenols and diethylstilbestrol in river water.