色谱最新文献

{"title":"[Determination of human serum total protein via electrophoresis titration and capacitively coupled contactless conductivity detection].","authors":"Rui-Hua Zhang, Ze-Hua Guo, Qiang Zhang, Gen-Han Zha, Cheng-Xi Cao, Liu-Yin Fan, Wei-Wen Liu","doi":"10.3724/SP.J.1123.2023.04015","DOIUrl":"10.3724/SP.J.1123.2023.04015","url":null,"abstract":"<p><p>Serum total protein refers to the sum of all proteins in the serum, and its content determination is relevant to human health monitoring and disease diagnosis. However, existing detection techniques present a number of limitations; for example, the Kjeldahl method suffers from the negative effects of interfering substances such as non-protein nitrogen (NPN). Although the electrophoresis titration (ET) method has solved interference problems to some extent, the current ET technique relies on optical detection methods, which increases the tediousness of the operation. This study addresses the challenge of accurate serum total protein detection by combining the traditional ET technique with capacitively coupled contactless conductivity detection (C<sup>4</sup>D). The research contributions of this work are multifold. First, it presents the first development of an ET-C<sup>4</sup>D detection system, which consists of six components: an ET power module, an ET chip, a C<sup>4</sup>D sensing module, a detection module, a data acquisition card, and software. The developed system can capture the conductivity of substances in the channel using the software developed by our laboratory during ET. The detection system can be used to quantify the total protein content in human serum without the addition of specific labeling reagents or using optical detection equipment, and its running time is approximately 300 s. Second, this research proposes the corresponding principle of the system. Under an electric field, ion migration results in different pH levels before and after the boundary, leading to a protein surface charge difference. The maintenance of the electrical neutrality of the substances in the detection channel is related to the protein surface charge; therefore, the ion concentration distribution of the substances in the detection channel changes as the protein surface charge varies. A plot of conductivity as a function of running time showed an \"inverted clock shape\", first falling and then rising. Owing to the addition of different types and concentrations of proteins, the microenvironment of the entire system changes, resulting in different changes in conductivity. Third, the performance of the detection system was tested using human serum albumin (HSA) standard protein, which was mixed with polyacrylamide gel (PAG) mother liquor, riboflavin, etc., and irradiated under ultraviolet light for 10 min to form a gel. The ET experiments were then carried out. The shape of the conductivity curve was consistent with the proposed principle, and the higher the HSA concentration, the lower the conductivity curve trough, followed by a lagged time of the trough. Quantitative analysis of the conductivity signals showed that the linear range was 0.25-3.00 g/L, with a linearity of up to 0.98. The limit of detection (LOD) was 0.01 g/L, the relative standard deviation (RSD) was 1.90%, and the relative error of the test values was <7.20%, indicating the good de","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 8","pages":"707-713"},"PeriodicalIF":1.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10398821/pdf/cjc-41-08-707.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9958860","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Chemical diversity of dissolved organic matter revealed by ultra performance liquid chromatography-Fourier transform ion cyclotron resonance mass spectrometry].","authors":"Chao Ma, Hong-Xing Ni, Yu-Lin Qi","doi":"10.3724/SP.J.1123.2023.03012","DOIUrl":"10.3724/SP.J.1123.2023.03012","url":null,"abstract":"<p><p>Dissolved organic matter (DOM) is a highly complex and heterogeneous mixture that exists in various environments, including rivers, oceans, soils, and atmospheric aerosols. DOM plays a crucial role in biogeochemical cycles and significantly influences the environment by regulating water quality, changing the climate, and transporting pollutants. Therefore, clarifying the detailed molecular composition of DOM is essential to obtain a better understanding of its physical and chemical properties, thereby enabling further elucidation of its biogeochemical behavior. In this study, Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) combined with quadrupole detection (QPD) was used to conduct the online ultra performance liquid chromatography (UPLC)-MS analysis of DOM in water, aerosol, and soil samples collected in Tianjin, China. The samples were extracted with pure water and filtered through a glass fiber membrane (0.45 μm). The DOM in the samples was then enriched by solid-phase extraction (SPE) and redissolved in water-acetonitrile (1∶1, v/v) at mass concentration of 200 mg/L for the LC-MS experiments. The mobile phases used for UPLC were water containing 0.1% (v/v) formic acid (A) and acetonitrile containing 0.1% (v/v) formic acid (B). The gradient elution procedure was as follows: 0-5 min, 0B; 5-11 min, 0B-95%B; 11-25 min, 95%B; 25-28 min, 95%B-0B; 28-30 min, 0B. The flow rate was 0.1 mL/min, and the injection volume was 10 μL. The UV wavelength was set at 274 nm. MS detection was performed in negative electrospray ionization (ESI(-)) mode with a capillary voltage of 5.0 kV, and the MS data were collected in broadband (<i>m/z</i> 150-1000) and QPD modes. The transient data size was set to 2M, the free induction decay signal length was 0.74 s, and the ion accumulation time was 0.030 s. Four chromatographic peaks were observed in the chromatograms. The first peak was identified as salt adduct compounds containing sodium formate. The three other peaks contained complex components, such as oxygen-rich, unsaturated tannin-like compounds, as well as low-oxygen, highly saturated lignin-like and protein/amino-like compounds. UPLC-FT-ICR MS was suitable for assigning the detailed elemental compositions of the DOM samples. UPLC effectively improved the ionization efficiency of difficult-to-ionize compounds and enhanced the detection accuracy of MS. Indeed, MS peaks with a mass difference of as small as 3.4 mDa were well identified. A total of 12027, 15593, and 8029 peaks in the mass spectra of the water, aerosol, and soil samples, respectively, were assigned to known elemental formulae. Peaks Ⅱ and Ⅲ were hydrophilic components mainly including CHNO and CHO compounds. Compared with peak Ⅱ, peak Ⅲ exhibited a significant increase in CHNOS and CHOS, indicating that UPLC exerted a certain separation effect on these compounds. Furthermore, the aerosol samples contained a higher concentration of sulfur-containing compounds than the wa","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 8","pages":"662-672"},"PeriodicalIF":1.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10398822/pdf/cjc-41-08-662.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9958857","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Application progress of hypercrosslinked porous organic polymers in cartridge-based solid phase extraction].","authors":"Tong-Tong Qin,&nbsp;Li Gao,&nbsp;Wen-Jie Zhao","doi":"10.3724/SP.J.1123.2022.12003","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.12003","url":null,"abstract":"<p><p>Hypercrosslinked porous organic polymers (HCPs), a novel type of porous materials synthesized via the Friedel-Crafts reaction, are widely used in gas storage, heterogeneous catalysis, chromatographic separation, and organic pollutant capture. HCPs have the advantages of a wide monomer source, low cost, mild synthesis conditions, and easy functionalization. In recent years, HCPs have shown great application potential in solid phase extraction. Given their high specific surface area, excellent adsorption properties, diverse chemical structures, and easy chemical modification, HCPs have been successfully applied to the extraction of different types of analytes with efficient extraction performance. Based on the chemical structure of HCPs, their target analytes, and the adsorption mechanism, HCPs can be classified as hydrophobic, hydrophilic, and ionic species. Hydrophobic HCPs are usually constructed as extended conjugated structures by overcrosslinking aromatic compounds as monomers. Common monomers include ferrocene, triphenylamine, triphenylphosphine, etc. This type of HCPs shows good adsorption effects on nonpolar analytes such as benzuron herbicides and phthalates through strong <i>π-π</i> and hydrophobic interactions. Hydrophilic HCPs are prepared by introducing polar monomers or crosslinking agents, or by modifying polar functional groups. This type of adsorbent is commonly used to extract polar analytes such as nitroimidazole, chlorophenol, tetracycline, etc. In addition to hydrophobic forces, polar interactions, such as hydrogen-bonding and dipole-dipole interactions, also occur between the adsorbent and analyte. Ionic HCPs are mixed-mode solid phase extraction materials formed by introducing ionic functional groups into the polymer. Mixed-mode adsorbents usually have a dual reversed-phase/ion-exchange retention mechanism, which helps control the retention behavior of the adsorbent by adjusting the elution strength of the eluting solvent. In addition, the extraction mode can be switched by controlling the pH of the sample solution and eluting solvent. In this manner, matrix interferences can be removed while the target analytes are enriched. Ionic HCPs present a unique advantage in the extraction of acid-base drugs in water. The combination of new HCP extraction materials with modern analytical techniques, such as chromatography and mass spectrometry, has been widely used in environmental monitoring, food safety, and biochemical analyses. In this review, the characteristics and synthesis methods of HCPs are briefly introduced, and the application progress of different types of HCPs in cartridge-based solid phase extraction is described. Finally, the future outlook of HCP applications is discussed.</p>","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"554-561"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311624/pdf/cjc-41-07-554.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10138283","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of kojic acid in fermented foods by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Dong-Yang Chen,&nbsp;Hao Zhang,&nbsp;Lei Zhang,&nbsp;Yi-Hong Wang,&nbsp;Xiao-Dan Wang,&nbsp;Jia-Li Feng,&nbsp;Jing Liang,&nbsp;Xuan Zhong","doi":"10.3724/SP.J.1123.2022.10002","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.10002","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Kojic acid naturally appears in fermented foods and can be formed during the aerobic fermentation process induced by &lt;i&gt;Aspergillus&lt;/i&gt; and &lt;i&gt;Penicillium fungi&lt;/i&gt;. It is widely used in the food industry because it exhibits antibacterial and antifungal properties and does not affect food taste. However, recent studies indicate that kojic acid may be a potential carcinogen. Therefore, assessing the health risks of kojic acid in fermented foods are of great importance, and developing a sensitive and accurate analytical method for this compound is a significant endeavor. Much efforts have been devoted to the detection of kojic acid using electrochemistry, high performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). HPLC and HPLC-MS/MS are the analytical techniques most often employed for this purpose. Of these two methods, HPLC-MS/MS displays excellent sensitivity and is the optimal selective technique. Pretreatment is usually necessary for kojic acid determination because of the complex matrix effects of fermented foods. However, few researches on the determination of kojic acid in food are available, and, to the best of our knowledge, the determination of kojic acid using solid-phase extraction (SPE) pretreatment has not been reported yet. Herein, a convenient, sensitive, and accurate method was developed to determine kojic acid in fermented foods using solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The pretreatment conditions, such as the extraction solvent, cartridge, rinse solvent, and eluent, were systematically optimized. The samples, including soy sauce, vinegar, liquor, sauce, fermented soya bean, and fermented bean curd, were extracted with 0.1% formic acid-absolute ethyl alcohol and purified using a PRiME HLB cartridge. Kojic acid was separated using an ACQUITY UPLC&lt;sup&gt;®&lt;/sup&gt; BEH C&lt;sub&gt;18&lt;/sub&gt; column (100 mm×2.1 mm, 1.7 μm) with formic acid-acetonitrile (1∶999, v/v) and formic acid-5 mmol/L ammonium acetate (1∶999, v/v) solutions as the mobile phases under gradient elution mode. MS was performed in electrospray positive ionization (ESI&lt;sup&gt;+&lt;/sup&gt;) and multiple reaction monitoring (MRM) modes. An internal standard method was used for quantification. Under optimized conditions, good linearity was achieved at mass concentrations of 5.0-100.0 μg/L, with a correlation coefficient (&lt;i&gt;r&lt;/i&gt;) of 0.9994. The limits of detection and quantification of the method for kojic acid were 2-5 μg/kg and 6-15 μg/kg, respectively. Good recoveries of 86.8%-111.7%, intra-day precisions of 1.0%-7.9% (&lt;i&gt;n&lt;/i&gt;=6), and inter-day precisions of 2.7%-10.2% (&lt;i&gt;n&lt;/i&gt;=5) were also obtained. The matrix effect was evaluated by establishing a matrix-matching calibration curve, and weak inhibitory effects were found in vinegar and liquor; moderate inhibitory effects in fermented bean curd, f","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"632-639"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311620/pdf/cjc-41-07-632.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10138287","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Recent application advances of covalent organic frameworks for solid-phase extraction].","authors":"Yi-Yang Gao, Ya-Li Ding, Lu-Yu Chen, Fang DU, Xu-Bo Xin, Juan-Juan Feng, Ming-Xia Sun, Yang Feng, Min Sun","doi":"10.3724/SP.J.1123.2022.12021","DOIUrl":"10.3724/SP.J.1123.2022.12021","url":null,"abstract":"<p><p>Covalent organic frameworks (COFs) are a type of crystalline porous polymers. It firstly prepared by thermodynamically controlled reversible polymerization to obtain chain units and connecting small organic molecular building units with a certain symmetry. These polymers are widely used in gas adsorption, catalysis, sensing, drug delivery, and many other fields. Solid-phase extraction (SPE) is a fast and simple sample pretreatment technology that can enrich analytes and improve the accuracy and sensitivity of analysis and detection; it is extensively employed in food safety detection, environmental pollutant analysis, and several other fields. How to improve the sensitivity, selectivity, and detection limit of the method during sample pretreatment have become a topic of great interest. COFs have recently been applied to sample pretreatment owing to their low skeleton density, large specific surface area, high porosity, good stability, facile design and modification, simple synthesis, and high selectivity. At present, COFs have also attracted extensive attention as new extraction materials in the field of SPE. These materials have been applied to the extraction and enrichment of diverse types of pollutants in food, environmental, and biological samples, such as heavy metal ions, polycyclic aromatic hydrocarbons, phenol, chlorophenol, chlorobenzene, polybrominated diphenyl ethers, estrogen, drug residues, pesticide residues, etc. COFs can be synthesized from different materials and exert different effects on different extracts. New types of COFs can also be synthesized via modification to achieve better extraction effects. In this work, the main types and synthesis methods of COFs are introduced, and the most important applications of COFs in the fields of food, environment and biology in recent years are highlighted. The development prospects of COFs in the field of SPE are also discussed.</p>","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"545-553"},"PeriodicalIF":1.2,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311619/pdf/cjc-41-07-545.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9761477","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of 41 veterinary drug residues in livestock and poultry meat using a composite purification system coupled with direct analysis in real time-tandem mass spectrometry].","authors":"Ying-Shuang Xie,&nbsp;Bo Wang,&nbsp;Chun-Ni Lei,&nbsp;Lan-Xia Liu,&nbsp;Huan Zhang,&nbsp;Xing-Bin Bai,&nbsp;Zong-Hong Kou","doi":"10.3724/SP.J.1123.2022.11022","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.11022","url":null,"abstract":"&lt;p&gt;&lt;p&gt;In a market environment where food safety problems still occur despite repeated prohibitions, food safety problems caused by veterinary drug residues and biological safety problems caused by the transfer of drug resistance have attracted much attention. Herein, a method based on a compound purification system coupled with direct analysis in real time-tandem mass spectrometry (DART-MS/MS) was established to determine 41 different types of veterinary drug residues in livestock and poultry products. First, a single-standard solution sampling method was used to optimize the selection of the best quasi-molecular ion, two daughter ions, and their cone-hole and collision voltages; qualitative and quantitative ion pairs are composed of a quasi-molecular ion and its corresponding daughter ion. The abundance ratios of the drug compounds in standard solutions of the solvent and matrix mixtures were then calculated according to the requirements of the European Union 2002/657 specification. DART-MS/MS was subsequently developed for the accurate characterization and quantitative analysis of the veterinary drugs. Finally, a composite purification pretreatment system was formed by combining the primary secondary amine (PSA) and octadecyl bonded silica gel (C18) of a QuEChERS technology with multiwalled carbon nanotubes (MWCNTs) to achieve the one-step purification of the drug compounds. The influence of the key parameters of the DART ion source on the determination of the drugs was investigated using the peak areas of the quantitative ions as the criterion. The optimum conditions were as follows: ion source temperature of 350 ℃, 12-Dip-it Samplers module, sample injection speed of 0.6 mm/s, and external vacuum pump pressure of -75 kPa. According to the differences in the dissociation constant (p&lt;i&gt;K&lt;/i&gt;&lt;sub&gt;a&lt;/sub&gt;) ranges of the 41 types of veterinary drug compounds and the characteristics of the sample matrixes, the extraction solvent, matrix-dispersing solvent, and purification method were optimized based on the recovery. The extraction solvent was 1.0% acetonitrile formate solution, and the pretreatment column included MWCNTs containing 50 mg of PSA and 50 mg of C18. The three chloramphenicol drugs showed a linear relationship in the ranges of 0.5-20 μg/L with correlation coefficients of 0.9995-0.9997,and the detection and quantification limits of three chloramphenicol drugs were 0.1 and 0.5 μg/kg, respectively. The 38 other drugs, including quinolones, sulfonamides, and nitro-imidazoles showed a linear relationship in the ranges of 2-200 μg/L with correlation coefficients of 0.9979-0.9999, and the detection and quantification limits of the 38 other drugs were 0.5 and 2.0 μg/kg, respectively. The recoveries of the 41 veterinary drugs at low, medium, and high spiked levels in chicken, pork, beef, and mutton samples were 80.0%-109.6%, with intra- and inter-day precisions of 0.3%-6.8% and 0.4%-7.0%, respectively. A total of 100 batches of animal meat (por","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"622-631"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311625/pdf/cjc-41-07-622.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9761478","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of catecholamines in urine by disperse solid-phase extraction-liquid chromatography based on Ti₃C₂T<i>_x</i>/polyimide composites].","authors":"Yuan-Qing Zhao,&nbsp;Kai Hu,&nbsp;Cheng Yang,&nbsp;Peng-Zhao Han,&nbsp;Li-Xin Li,&nbsp;Xiao-Bing Liu,&nbsp;Zhen-Qiang Zhang,&nbsp;Shu-Sheng Zhang","doi":"10.3724/SP.J.1123.2022.09004","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.09004","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Neurotransmitters (NTs) are basic signaling chemicals used for communication between cells. The most well-known catecholamines (CAs) are epinephrine, norepinephrine, and dopamine. CAs are an important class of monoamine NTs that contain catechins and amine groups. The accurate determination of CAs in biological samples can provide essential information on potential pathogenic mechanisms. However, biological samples generally contain only trace levels of CAs. Therefore, sample pretreatment is necessary to separate and enrich CAs before instrument analysis. Dispersive solid-phase extraction (DSPE) technology combines the principles of liquid-liquid extraction and solid-phase extraction and is a useful method for purifying and enriching the target analytes in complex matrices. This method has the advantages of low solvent consumption, environmental safety, and high sensitivity and efficiency. In addition, the adsorbents used in DSPE do not need to be packed into a column and can simply be completely dispersed in the sample solution; this excellent feature greatly improves the extraction efficiency and simplifies the extraction process. Therefore, the development of new DSPE materials with high efficiency and adsorption capacity using simple preparation procedures has received wide attention from the research community. Carbon nitrides (MXenes) are a class of two-dimensional layered materials that possess good hydrophilicity, a large number of functional groups (-O, -OH, and -F), large layer spacing, different elemental compositions, excellent biocompatibility, and environmental friendliness. However, these materials have a small specific surface area and poor adsorption selectivity, which limits their applications in SPE. The separation selectivity of MXenes can be significantly improved by functional modification. Polyimide (PI) is a crosslinking product that is mainly formed by the condensation polymerization of binary anhydride and diamine. It has a unique crosslinked network structure, as well as a large number of carboxyl groups, and shows excellent characteristics. Therefore, the synthesis of new PI-functionalized Ti&lt;sub&gt;3&lt;/sub&gt;C&lt;sub&gt;2&lt;/sub&gt;T&lt;i&gt;&lt;sub&gt;x&lt;/sub&gt;&lt;/i&gt; (Ti&lt;sub&gt;3&lt;/sub&gt;C&lt;sub&gt;2&lt;/sub&gt;T&lt;i&gt;&lt;sub&gt;x&lt;/sub&gt;&lt;/i&gt;/PI) composites by growing a PI layer on the surface of two-dimensional MXene nanosheets in situ may not only overcome the adsorptive limitations of MXenes but also effectively improve their specific surface area and porous structure, thereby enhancing their mass transfer capacity, adsorption capacity, and selectivity. In this study, a Ti&lt;sub&gt;3&lt;/sub&gt;C&lt;sub&gt;2&lt;/sub&gt;T&lt;i&gt;&lt;sub&gt;x&lt;/sub&gt;&lt;/i&gt;/PI nanocomposite was fabricated and successfully applied as a DSPE sorbent to enrich and concentrate trace CAs in urine samples. The prepared nanocomposite was examined using various characterization methods, including scanning electron microscopy, Fourier transform-infrared spectroscopy, X-ray diffraction, and zeta potential analysis. The effects of the ","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"572-581"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311628/pdf/cjc-41-07-572.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9761482","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[One-pot synthesis of a poly(styrene-acrylic acid) copolymer-modified silica stationary phase and its applications in mixed-mode liquid chromatography].","authors":"Xiao-Qing Wang,&nbsp;Jian Cui,&nbsp;Yi-Ming Gu,&nbsp;Shuo Wang,&nbsp;Jin Zhou,&nbsp;Shu-Dong Wang","doi":"10.3724/SP.J.1123.2023.01005","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2023.01005","url":null,"abstract":"&lt;p&gt;&lt;p&gt;As modified ligands with a wide range of sources, abundant functional groups, and good biocompatibility, polymers have been widely used in the development of silica-based chromatographic stationary phases. In this study, a poly(styrene-acrylic acid) copolymer-modified silica stationary phase (SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA)) was prepared via one-pot free-radical polymerization. In this stationary phase, styrene and acrylic acid were used as functional repeating units for polymerization and vinyltrimethoxylsilane (VTMS) was used as a silane coupling agent to link the copolymer and silica. Various characterization methods, such as Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), N&lt;sub&gt;2&lt;/sub&gt; adsorption-desorption analysis, and Zeta potential analysis, confirmed the successful preparation of the SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA) stationary phase, which had a well-maintained uniform spherical and mesoporous structure. The retention mechanisms and separation performance of the SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA) stationary phase in multiple separation modes were then evaluated. Hydrophobic and hydrophilic analytes as well as ionic compounds were selected as probes for different separation modes, and changes in the retention of the analytes under various chromatographic conditions, including different methanol or acetonitrile contents and buffer pH values, were investigated. In reversed-phase liquid chromatography (RPLC) mode, the retention factors of alkyl benzenes and polycyclic aromatic hydrocarbons (PAHs) on the stationary phase decreased with increasing methanol content in the mobile phase. This finding could be attributed to the hydrophobic and &lt;i&gt;π-π&lt;/i&gt; interactions between the benzene ring and analytes. The retention changes of alkyl benzenes and PAHs revealed that the SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA) stationary phase, similar to the C18 stationary phase, exhibited a typical reversed-phase retention behavior. In hydrophilic interaction liquid chromatography (HILIC) mode, as the acetonitrile content increased, the retention factors of hydrophilic analytes gradually increased, and a typical hydrophilic interaction retention mechanism was inferred. In addition to hydrophilic interaction, the stationary phase also demonstrated hydrogen-bonding and electrostatic interactions with the analytes. Compared with the C18 and Amide stationary phases prepared by our groups, the SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA) stationary phase exhibited excellent separation performance for the model analytes in the RPLC and HILIC modes. Owing to the presence of charged carboxylic acid groups in the SiO&lt;sub&gt;2&lt;/sub&gt;@P(St-b-AA) stationary phase, exploring its retention mechanism in ionic exchange chromatography (IEC) mode is of great importance. The effect of the mobile phase pH on the retention time of organic bases and acids was further studied to explore the electrostatic interaction between the stationary phase and charged analy","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"562-571"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311627/pdf/cjc-41-07-562.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9761479","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[High-throughput screening of multi-pesticide residues in animal-derived foods by QuEChERS-online gel permeation chromatography-gas chromatography-tandem mass spectrometry].","authors":"Jie Li,&nbsp;Xiang Ju,&nbsp;Yan-Li Wang,&nbsp;Qi-Yan Tian,&nbsp;Xiu-Qing Liang,&nbsp;Hai-Xia Li,&nbsp;Yan-Ming Liu","doi":"10.3724/SP.J.1123.2022.10010","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.10010","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Improvements in living standards have led to an increase in the consumption of animal-derived foods. Pesticides may be used illegally during animal breeding as well as meat production and processing for pest control and preservation. Pesticides applied to crops may also be enriched in animal tissues through the food chain, thereby increasing the risk of pesticide residue accumulation in muscles and visceral tissues and endangering human health. China has stipulated maximum residue limits for pesticide residues in livestock and poultry meat and their viscera. Many other major developed countries and organizations, including the European Union, Codex Alimentarius Commission, and Japan, have also set maximum residue limits for these residues (0.005-10, 0.004-10, and 0.001-10 mg/kg, respectively). Research on pretreatment technologies for pesticide residue detection in plant-derived foods is widely available, but insufficient attention has been paid to animal-derived foods. Thus, high-throughput detection technologies for pesticide residues in animal-derived foods are limited. The impurities that can interfere with the detection process for plant-derived foods mainly include organic acids, polar pigments, and other small molecular compounds; by contrast, the matrix of animal-derived foods is much more complex. Macromolecular proteins, fats, small molecular amino acids, organic acids, and phospholipids can interfere with the detection of pesticide residues in animal-derived foods. Thus, selecting the appropriate pretreatment and purification technology is of great importance. In this study, the QuEChERS technique was combined with online gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS/MS) to determine 196 pesticide residues in animal-derived foods. The samples were extracted with acetonitrile, purified using the QuEChERS technique coupled with online GPC, detected by GC-MS/MS, determined in multiple reaction monitoring mode (MRM), and quantified using the external standard method. The effects of the extraction solvent and purification agent type on the extraction efficiency and matrix removal of the method were optimized. The purification effect of online GPC on the sample solution was investigated. The optimal distillate receiving time was obtained by studying the recoveries of the target substances and matrix effects over different distillate receiving periods to achieve the effective introduction of target substances and efficient matrix removal. Further, the advantages of the QuEChERS technique combined with online GPC were evaluated. The matrix effects of 196 pesticides were assessed; ten pesticide residues showed moderate matrix effects, while four pesticide residues showed strong matrix effects. A matrix-matched standard solution was used for quantification. The 196 pesticides showed good linearity in the range of 0.005-0.2 mg/L, with correlation coefficients greater than 0.996. The limits of detection","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"610-621"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311622/pdf/cjc-41-07-610.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10138284","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of bisphenols in sediment by accelerated solvent extraction and solid-phase extraction purification coupled with ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Qiu-Xu Wang,&nbsp;Qi-Yan Feng,&nbsp;Xue-Qiang Zhu","doi":"10.3724/SP.J.1123.2022.12015","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.12015","url":null,"abstract":"<p><p>Bisphenols are endocrine disruptors that are characterized with bioaccumulation, persistence, and estrogenic activity. Even low contents of bisphenols can exert adverse effects on human health and the ecological environment. Herein, a method combining accelerated solvent extraction and solid-phase extraction purification with ultra performance liquid chromatography-tandem mass spectrometry was developed for the accurate detection of bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF), bisphenol S (BPS), bisphenol Z (BPZ), bisphenol AF (BPAF), and bisphenol AP (BPAP) in sediments. The mass spectrometric parameters of the seven bisphenols were optimized, and the response values, separation effects, and chromatographic peak shapes of the target compounds were compared under three different mobile phase conditions. The sediment samples were pretreated by accelerated solvent extraction, and orthogonal tests were used to optimize the extraction solvent, extraction temperature, and cycle number. The results showed that the use of 0.05% (v/v) ammonia and acetonitrile as the mobile phase for gradient elution could rapidly separate the seven bisphenols on an Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm). The gradient program was as follows: 0-2 min, 60%A; 2-6 min, 60%A-40%A; 6-6.5 min, 40%A; 6.5-7 min, 40%A-60%A; 7-8 min, 60%A. Orthogonal experiments indicated that the optimal extraction conditions were as follows: extraction solvent of acetonitrile, extraction temperature of 100 ℃, and cycle number of three. The seven bisphenols showed good linearity in the range of 1.0-200 μg/L, with correlation coefficients (<i>r</i>²) greater than 0.999, and the limits of detection were 0.01-0.3 ng/g. The recoveries for the seven bisphenols ranged from 74.9% to 102.8% at three spiking levels (2.0, 10, 20 ng/g), with relative standard deviations ranging from 6.2% to 10.3%. The established method was applied to detect the seven bisphenols in sediment samples collected from Luoma Lake and its inflow rivers. BPA, BPB, BPF, BPS, and BPAF were detected in the sediments of the lake, and BPA, BPF, and BPS were detected in the sediments of its inflow rivers. The detection frequency of BPA and BPF was 100%, and the contents of these bisphenols in the sediment were 11.9-38.0 ng/g and 11.0-27.3 ng/g, respectively. The developed method is simple, rapid with high accuracy and precision, and is suitable for the determination of the seven bisphenols in sediment.</p>","PeriodicalId":9864,"journal":{"name":"色谱","volume":"41 7","pages":"582-590"},"PeriodicalIF":0.7,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10311623/pdf/cjc-41-07-582.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10138286","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}