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Chinese Journal of Chromatography
2020, Vol. 38, No. 3
Online: 08 March 2020

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Volume 38, Number 3 Content 2020, 38 (3):  0-0.  Abstract ( 23 )   PDF (4937KB) ( 18 )

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Applications of molecularly imprinted polymers for determination of antibiotics residues WANG Liyan, WANG Jia'nan, LI Jinhua, CHEN Lingxin 2020, 38 (3):  265-277.  DOI: 10.3724/SP.J.1123.2019.07007 Abstract ( 179 )   HTML ( 17 )   PDF (3582KB) ( 116 )   Abuse of antibiotics as well as antibiotic residues cause great harm to living beings and the environment. However, determination of antibiotics is quite difficult owing to the low residue level and multiple categories presence in the complicated matrices. Proper sample pretreatment is usually imperative for coupling with chromatographic analysis toward the sensitive determination of antibiotic residues. Molecularly imprinted polymers (MIPs) possess the binding sites complementary to the target (template) molecules in shape, size, and type of functional groups. Hence, MIPs can selectively recognize and effectively enrich the target analytes as well as eliminate matrix interferences. For this reason, they have been widely applied in the sample pretreatment of antibiotics. In this review, several challenges encountered with the use of MIPs and the possible solutions are proposed. Besides, advances in the applications of MIPs for the sample pretreatment of antibiotics since 2016 are summarized, mainly including conventional solid phase extraction (SPE), dispersive solid phase extraction (DSPE), magnetic solid phase extraction (MSPE), matrix solid phase dispersion (MSPD), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). Some new imprinting strategies for the preparation of MIPs to be used in the field of antibiotics are highlighted, such as multi-template imprinting, multi-functional monomer imprinting, dummy imprinting, stimuli-responsive imprinting and hydrophilic imprinting. Finally, an outlook on the preparation and pretreatment application of MIPs for antibiotics is presented.

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Advancesin enrichment and detection methods for N-phosphorylated proteins HU Yechen, JIANG Bo, ZHANG Lihua, ZHANG Yukui 2020, 38 (3):  278-286.  DOI: 10.3724/SP.J.1123.2019.09015 Abstract ( 138 )   HTML ( 11 )   PDF (2559KB) ( 80 )   Protein phosphorylation plays an important role in various life processes, such as signaling, metabolism, and growth. In addition to the well-known O-phosphorylation, which occurs on serine, threonine and tyrosine side chains, N-phosphorylation, occurring on histidine, arginine and lysine side chains, has attracted much attention. However, due to the chemical instability of N-phosphorylation, the studies on it are still in the nascent stage. In this review, enrichment and detection methods for protein N-phosphorylation are reviewed, and future research in this field is prospected.

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Research progress on the analytical method of perfluoroalkyl and polyfluoroalkyl substances HE Sisi, SHI Yali, CAI Yaqi, ZHANG Chunhui 2020, 38 (3):  287-296.  DOI: 10.3724/SP.J.1123.2019.09019 Abstract ( 355 )   HTML ( 31 )   PDF (875KB) ( 196 )   With the gradual implementation of the Stockholm Convention on persistent organic pollutants (POPs), perfluoroalkyl and polyfluoroalkyl substances (PFASs) have attracted more extraordinary attentions from environmental researchers. Researches into the environmental persistence, toxicity and bioaccumulative potential of PFASs have entered a new stage of rapid development owing to their massive detection in various environmental media. Because of the regulatory limitations on legacy PFASs, their isomers and precursors, and various emerging PFASs as their substituents have been concerned by many scientists and organizations. Till date, numerous methods for the sample pretreatment and analysis of diverse PFASs have been proposed, which have distinctive advantages. Hence, appropriate choice of the analytical method is imperative for studying the environmental behavior and fate of PFASs, even for precautionary environmental management. This paper reviews the research progress on pretreatment and analytical methods, including HPLC-MS, GC-MS and HPLC-high resolution mass spectrometry (HRMS), GC-HRMS, used for the determination of legacy PFASs as well as, their isomers and precursors, and emerging PFASs. The current problems and critical areas of research that warrant further attention are also discussed herein.

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Research advances in supramolecular macrocyclic compounds for dye adsorption LI Ping, ZHANG Dawei, JIA Qiong 2020, 38 (3):  297-306.  DOI: 10.3724/SP.J.1123.2019.10018 Abstract ( 91 )   HTML ( 8 )   PDF (1094KB) ( 42 )   Dyes have long been used in many industrial fields, and this has led to severe environmental water pollution, eventually posing a threat to human health. Therefore, effective removal of dyes from water is an urgent problem to be addressed. Adsorption is one of the most attractive techniques for reducing the dye content in water because of its high efficiency, simplicity, and low cost. The choice of adsorbent is critical for the efficient adsorption of dyes. Macrocyclic compounds with a large cavity as a host molecule show a strong adsorption effect on many guest molecules and have thus attracted attention as dye adsorbents. In this paper, the preparation of macrocyclic compound-based adsorbents and their applications in the removal of dyes in water are reviewed. The adsorption performance of various adsorbents are discussed, and their future development is proposed.

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Advances on preparation methods for mycotoxins in food samples HU Wenyao, LONG Meiming, HU Yufei, LI Gongke 2020, 38 (3):  307-316.  DOI: 10.3724/SP.J.1123.2019.10023 Abstract ( 175 )   HTML ( 14 )   PDF (1499KB) ( 90 )   Mycotoxins are toxic secondary metabolites with low molecular weight that are produced by fungus under certain environmental conditions. Mycotoxins are of various types and show strong toxicity. They can enter the food chain directly or indirectly, causing diseases or even death to humans and other animals. It is very crucial to use efficient sample preparations to realize the separation and enrichment of targets before analysis due to diversified foods, complex matrix and low concentrations in real samples. In this paper, preparation methods using new separation media, such as liquid phase extraction, solid phase extraction, magnetic solid phase extraction, ultrasound-assisted extraction, microwave-assisted extraction, immunoaffinity chromatography and QuEChERS are introduced. In addition, future trends in sample preparation for food mycotoxins are prospected.

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Recent advances of separation and analysis of chiral compounds by capillary electrophoresis LIU Mingxia, LI Xiangjun, BAI Yu, LIU Huwei 2020, 38 (3):  317-323.  DOI: 10.3724/SP.J.1123.2019.10019 Abstract ( 252 )   HTML ( 22 )   PDF (847KB) ( 162 )   As the enantiomers of chiral compounds often exhibit different physiological activities, the establishment of effective separation and analytical methods for chiral compounds is of great significance. As a widely used chiral separation and detection technique, capillary electrophoresis (CE) offers the advantages of high separation efficiency, high speed, small sample consumption and flexible separation mode. In this review, research progresses in chiral separation by CE for the period 2017 to 2019 are summarized, and future developments are prospected.

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Monitoring chemical synthesis of human atrial natriuretic peptide by ultra high performance liquid chromatography-mass spectrometry analysis XU Kun, JIN Yulong, HUANG Yanyan, ZHAO Rui 2020, 38 (3):  324-331.  DOI: 10.3724/SP.J.1123.2019.10020 Abstract ( 101 )   HTML ( 8 )   PDF (1380KB) ( 41 )   Peptides participate in and regulate many important life processes as neurotransmitters, hormones and receptors. With detailed understanding of the structure and function of peptides, chemically synthesized peptides have shown great value in the fields of biomedicine and life analysis. Human atrial natriuretic peptide (ANP) is a polypeptide hormone consisting of 28 amino acids. The abnormalities in the content and metabolism of ANP are closely related to the diseases like cardiovascular diseases and cancer. In view of the important physiological functions of ANP, herein we monitored and optimized the chemical synthesis of ANP chemical synthesis. The strategy involved integrating solid phase synthesis of linear peptide chain and liquid phase oxidation. Based on the excellent separation performance of HPLC and the excellent qualitative ability of mass spectrometry (MS), a new method based on ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established to monitor the synthesis reaction and to separate and purify the obtained products. This study provides a reference for the efficient chemical synthesis and oxidative ring formation of human atrial natriuretic peptide.

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In-situ solvothermal polymerization of metal-organic framework/carbon-nitrogen nanosheet-coated solid-phase microextraction fiber for highly sensitive detection of pesticide residues in black tea ZHANG Wenmin, FENG Zunmei, HUANG Chuanhui, GAO Jia, ZHANG Lan 2020, 38 (3):  332-340.  DOI: 10.3724/SP.J.1123.2019.10036 Abstract ( 102 )   HTML ( 5 )   PDF (4080KB) ( 57 )   Pyrethroids (PYs) and organochlorine pesticides (OCPs) are widely used to control pests and diseases in plants; however, they threaten human health. In this study, a metal-organic framework/carbon-nitrogen nanosheet composite nanomaterial (UiO-66/HOCN)-coated solid-phase microextraction (SPME) fiber was prepared by in-situ thermal polymerization. The prepared UiO-66/HOCN composite material was characterized by transmission electron microscopy, X-ray diffraction, nitrogen adsorption porosimetry, thermogravimetric analysis, and zeta potentiometry. The prepared UiO-66/HOCN composite-coated MSPE fiber was used for the enrichment and separation of OCPs and PYs, which showed good thermal and chemical stability as well as high extraction efficiency. Combined with gas chromatography-mass spectrometry (GC-MS), an efficient and sensitive method for the detection of trace levels of OCPs and PYs was developed. Under the optimal experimental conditions, wide linear ranges (0.1-800.0 ng/L), good linearity (≥ 0.9978), low limits of detection (0.03-0.30 ng/L), and acceptable repeatability (RSD ≤ 8.9%, n=3) were obtained. Typical black tea samples were analyzed by the developed method, and trace levels of aldrin (6.6 ng/g), α -endosulfan (54.7 ng/g), and bifenthrin (185.8 ng/g) were detected. The results demonstrate that the developed method has immense potential for the detection of pesticides in a complicated matrix.

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Preparation of seven kinds of amino bonded silica gels and their adsorption to heavy metal Pb2+ LI Laiming, REN Fangfang, ASSEFA Aschenaki, LIU Jia, ZHANG Xiaofei, BAO Jianmin, LI Youxin 2020, 38 (3):  341-349.  DOI: 10.3724/SP.J.1123.2019.09030 Abstract ( 103 )   HTML ( 9 )   PDF (7507KB) ( 51 )   Seven kinds of amino bonded silica gels were prepared. They were aminopropyl bonded silica gel (SiO2-N), ethylenediamine-N-propyl bonded silica gel (SiO2-2N), diethylenetriamine bonded silica gel (SiO2-3N), triethylenetetramine bonded silica gel (SiO2-4N), tetraethylene pentamine bonded silica gel (SiO2-5N), pentaethylene hexamine bonded silica gel (SiO2-6N) and polyvinylimide bonded silica gel (SiO2-nN). The densities of the bonded amino groups in SiO2-N and SiO2-2N prepared by a one-step method were up to 2.07mmol/g and 1.71mmol/g, respectively. The density of the bonded amino groups in SiO2-nN with ethylene imine units prepared by a two-step method, was 0.02mmol/g. The densities of the bonded amino groups in the other silica gels were similar, about 0.50mmol/g. The synthesized silica gels were used to investigate the adsorption of the heavy metal ion Pb2+ which commonly exists in aqueous solutions. About 20 mg of the silica gel was added to 10 mL of 400 mg/L Pb2+, at pH 5 and 30℃. The results indicated that the adsorption capacity reached the maximum value after 10 h. The adsorption process was fit to the Freundlich isothermal equation. The adsorption capacities of SiO2-N, SiO2-2N, SiO2-3N, SiO2-4N, SiO2-5N, SiO2-6N and SiO2-nN to Pb2+were 131.28, 138.98, 85.37, 75.22, 61.87, 79.12 and 114.06 mg/g, respectively, indicating the potential utility of these amino-functionalized silica gels for the adsorption of Pb2+.

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Application of porous layer open tubular capillary columns with narrow inner diameter in nanoflow-high performance liquid chromatography for N-derivatized amino acid enantiomers LI Ruonan, WANG Lijuan, ZHANG Dongtang, WANG Yanan, GUO Guangsheng, WANG Xiayan 2020, 38 (3):  350-355.  DOI: 10.3724/SP.J.1123.2019.09002 Abstract ( 92 )   HTML ( 7 )   PDF (3735KB) ( 97 )   Porous layer open tubular capillary columns with a narrow inner diameter (NPLOT) have potential in life science, especially in single-cell analysis. In this work, quinidine-based chiral NPLOT columns were prepared by in-situ thermal-initiated polymerization. The porous layer of the organic polymer was prepared with a 6 μm i. d capillary by in-situ thermal-initiated polymerization, following which the thickness and morphology of the NPLOT column were observed for different durations (3 h, 6 h, and 9 h) of polymerization. The thicknesses of the porous layer were 103±51 nm and 210±51 nm when polymerization was conducted for 3 h and 6 h, respectively. Subsequently, the columns prepared under 3 h of polymerization were applied in nanoflow-high performance liquid chromatography for the enantioseparation of N-derivatized amino acid enantiomers. Baseline separation was achieved in 2 min. The sample volume consumed was of the picoliter level, which would provide a means of research for single-cell analysis.

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Simultaneous determination of inorganic anions and cations in wine by capillary electrophoresis-indirect ultraviolet detection with ionic liquid as background electrolyte TIAN Miaomiao, LIU Xin, YANG Li 2020, 38 (3):  356-361.  DOI: 10.3724/SP.J.1123.2019.09010 Abstract ( 96 )   HTML ( 7 )   PDF (1119KB) ( 56 )   A novel method was developed for the simultaneous determination of inorganic anions (Cl-, SO42- and ClO3-) and cations (K+, Ca2+, Na+, Mg2+ and Li+) in wine by capillary electrophoresis-indirect ultraviolet detection (CE-UV) with dual-opposite end injection using 1-ethyl-3-methylimidazolium p-toluenesulfonate ([EMIm]TS) as the background electrolyte.[EMIm]TS acted as the running electrolyte and probe, generating the background signals for cations and anions under indirect UV light, consequently simplifying the electrophoretic medium. Under the optimal experimental conditions, baseline separation was achieved for the eight inorganic ions within 6.5 min. The linear ranges of the eight inorganic ions were 0.005-0.7 g/L, with correlation coefficients (R2) of 0.963-0.995. The limits of detection (LODs) were between 1.2 and 12.5 mg/L at a signal-to-noise ratio of 3 (S/N=3). Eight inorganic ions were detected in three different brands of wines obtained from supermarket. Good recoveries of 90.1%-110.5% at three spiked levels (0.05, 0.2 and 0.4 g/L) were achieved with a low relative standard deviations (RSDs) (n=5) of 1.1%-4.8%. The proposed method is robust and reliable for the sensitive and rapid analysis of the inorganic anions and cations, and it has potential in evaluating the quality of wine.