Se pu = Chinese journal of chromatography最新文献

{"title":"[Determination of 30 bile acids in the bile of <i>Micropterus salmoides</i> and <i>Ctenopharyngodon idella</i> using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry].","authors":"Ling-Wen Mao, Hao Sun, Hai-Jie Chen, Qian-Zhan Yang, Lan Xu","doi":"10.3724/SP.J.1123.2024.03004","DOIUrl":"10.3724/SP.J.1123.2024.03004","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Bile acids (BAs), the primary components of bile, play significant roles in sugar, lipid, and cholesterol metabolism. Normal BA metabolism maintains a dynamic equilibrium by regulating gut microbiota to effectively protect the liver and intestines, thereby sustaining overall health. Conversely, abnormal BA metabolism can cause intestinal tissue and liver damage, disruption of enterohepatic circulation homeostasis, dysbiosis of gut microbiota, and gastrointestinal and hepatic diseases. Although largemouth bass (&lt;i&gt;Micropterus salmoides&lt;/i&gt;) and grass carp (&lt;i&gt;Ctenopharyngodon idella&lt;/i&gt;) are important freshwater fish species in China, their BA profiles have not been fully characterized. Elucidating these profiles could provide valuable data to support the aquaculture industry. In this study, a qualitative and quantitative method for the simultaneous determination of 30 BAs in the gallbladders of &lt;i&gt;M. salmoides&lt;/i&gt; and &lt;i&gt;C. idella&lt;/i&gt; was developed using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry. The samples were centrifuged and then the supernatant was extracted, vortex-mixed with methanol, and filtered through a 0.22 μm membrane. Various mobile phase systems commonly used in liquid chromatography-mass spectrometry were investigated, including formic acid, acetic acid, ammonium formate, acetic acid-ammonium, and methanol-acetonitrile. Based on the response intensity, chromatographic separation, and peak shape of each substance, the optimal mobile phase was acetic acid and acetonitrile, and the concentration of acetic acid in water was optimized. To improve the ionization efficiency, the most effective ion scanning mode was selected by comparing the response intensities and peak conditions of each BA during mass spectrometry in positive and negative ion modes. Furthermore, the interface voltage for each BA and the ion source interface temperature were investigated to determine the optimal mass spectrometry conditions. Ultimately, separation was performed using a Shim-pack Velox SP-C18 column (100 mm×2.1 mm, 1.8 μm) with gradient elution of 0.01% acetic acid aqueous solution and acetonitrile, and the total analysis time was 14 min. The column temperature was 50 ℃ and the injection volume was 2 μL. Multiple reaction monitoring of 8 positive ions and 22 negative ions was carried out using electrospray ionization. Different series of mixed standard working solutions, prepared based on the response intensity of each BA, were used to construct standard curves. All 30 BAs exhibited good linearities within the investigated concentration ranges, with correlation coefficients (&lt;i&gt;R&lt;/i&gt;&lt;sup&gt;2&lt;/sup&gt;) of 0.9975-0.9997, indicating high accuracy. Spiked recoveries were 72.3%-117.2%, and the inter-day precisions were in the range of 0.46%-13.23%. The limits of detection and quantification were 0.01-0.75 ng/mL and 0.02-2.28 ng/mL, respectively, enabling the precise detection of low-concentration BAs. Using the establis","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"220-227"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883528/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569195","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of vitamin D and 25-hydroxyvitamin D in animal-derived foods by derivatization-ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Yu Liu, Ji-Hui Xie, Ping-Ping Zhang, Di Zhou, Wei-Ke Zhao, Ju-Zhou Zhang","doi":"10.3724/SP.J.1123.2024.02003","DOIUrl":"10.3724/SP.J.1123.2024.02003","url":null,"abstract":"<p><p>Animal-derived foods are essential sources of vitamin D and 25-hydroxyvitamin D in the human diet. Currently, the relevant regulatory methods in China are limited to using non-derivatization methods to determine vitamin D content. In this study, 4-phenyl-1,2,4-triazoline-3-5-dione (PTAD) was used as a derivative reagent, and the ionization efficiencies of vitamin D and 25-hydroxyvitamin D were improved by introducing readily ionizable groups via the Diels-Alder reaction. This method allowed for the simultaneous determination of vitamin D and 25-hydroxyvitamin D in animal-derived foods using derivatization and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The conditions for derivatization, sample pretreatment, chromatographic separation, and MS detection were optimized. The results showed that the derivatization reaction was effective in acetonitrile solvent at a target compound to PTAD mass ratio of 1∶10000 and stabilized after 1 h. Compared with Silica and C₁₈ solid-phase extraction (SPE) columns, hydrophilic lipophilic balanced (HLB) SPE columns yielded higher recoveries of the target compounds, while simultaneously reducing the matrix effect. The detection sensitivity was significantly improved by adding 5 mmol/L methylamine to the water-methanol mobile phase system. An isotopic internal standard was added to the homogenized samples, which were saponified with alkali solution, extracted and concentrated, purified using a SPE column, derivatized, and separated on a Waters Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm) with a gradient elution using 0.1% formic acid-5 mmol/L methylamine aqueous solution and 0.1% formic acid-5 mmol/L methylamine of methanol as the mobile phases. The analytes were determined by multiple reaction monitoring (MRM) in positive electrospray ionization mode (ESI⁺) and quantified using the internal standard method. The results for both vitamin D and 25-hydroxyvitamin D showed good linearity in the range of 0.2-50 μg/L, with correlation coefficients of 0.9995-0.9999. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.018-0.066 and 0.06-0.22 μg/kg, respectively. Recoveries were 92.6%-99.4% at three spiked levels (0.20, 1.0, and 5.0 μg/kg), and the relative standard deviations (RSDs) were 3.6%-6.2%. This highly sensitive method yields reproducible and accurate results for the quantitative determination of vitamin D and 25-hydroxyvitamin D in animal-derived foods.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"228-236"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883526/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569255","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of 17 perfluorinated/polyfluoroalkyl compounds in serum by high-throughput solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry].","authors":"Qiang Lin, Jian Wang, Jing-Jing Li, Dong-Xia Su, Mei-Li Li, Jia Wang, Yu-Min Niu, Bing Shao","doi":"10.3724/SP.J.1123.2024.03007","DOIUrl":"10.3724/SP.J.1123.2024.03007","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Perfluorinated/polyfluoroalkyl compounds (PFASs) are a group of synthetic chemicals. Since the 1940s, PFASs have been widely used in industrial and daily consumer fields. PFASs can enter the human body through various pathways, such as drinking water, food, and air. Toxicological studies have shown that PFASs feature developmental and reproductive toxicity. Thus, the accurate assessment of PFAS exposure levels plays an important role in determining the health risks of these compounds. Biological monitoring is considered the most ideal means of monitoring and evaluating PFAS levels in the human body. The concentration of PFASs in serum can directly reflect their level of absorption in the human body after exposure; therefore, serum is widely used as a biological matrix for evaluating PFASs. In this study, a high-throughput solid-phase extraction (SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed for the determination of 17 PFASs in serum. A laboratory-made straight-through SPE column was used to purify serum samples. The SPE column used a new inorganic material with a low perfluorinated compound background. Unlike traditional SPE columns, the extraction column does not require activation before use, and the sample can be directly loaded into it for purification. The straight-through SPE column adopts a stepped design, which does not require a large sample volume and is suitable for the pretreatment of precious biological samples such as serum. The serum sample size adopted in this study was only 50 μL, which is much lower than that required by other extraction methods. The straight-through SPE column can be used in conjunction with a 96-well plate, and the purification treatment of 96 serum samples can be completed within 30 min with high efficiency. The mass spectrometry parameters were optimized, and the results indicated that the electrospray ionization source temperature had a significant impact on the PFASs with later elution peaks. The effects of ion-source temperatures of 400 and 500 ℃ on the peak shapes and response values of the target compounds were compared, and 400 ℃ was selected. The sample pretreatment and ultra-high performance liquid chromatographic conditions were optimized. Briefly, 50 μL of the sample was loaded into the SPE column and extracted twice using 200 μL of acetonitrile each time. The purified solution was collected, blown with nitrogen at 40 ℃ to near dryness, dissolved in a 50% methanol aqueous solution, and then separated on a Poroshell 120 EC-C18 chromatographic column (100 mm×3 mm, 2.7 μm) with 5 mmol/L ammonium acetate aqueous solution and methanol as mobile phases. Detection was conducted in multiple-reaction monitoring mode, and quantification was performed using an isotope internal standard method. The 17 detected PFASs had good linear relationships within the corresponding mass concentration ranges (&lt;i&gt;r&lt;/i&gt;&lt;sup&gt;2&lt;/sup&gt;&gt;0.995), with limits of detectio","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"252-260"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883548/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569189","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Simultaneous determination of six polyhydroxyl compounds in cosmetics and toothpaste using high performance liquid chromatography with evaporative light-scattering detection].","authors":"Shu'e Zhao, Lu Yuan, Dan-Dan Liao, Xiang Luo, Geng-Peng Xiao","doi":"10.3724/SP.J.1123.2024.02019","DOIUrl":"10.3724/SP.J.1123.2024.02019","url":null,"abstract":"<p><p>With the full implementation of the cosmetic formula ingredient registration system and the standardized management of labels and identification, the ingredients registered and declared on the label must be consistent with the actual ingredients contained in the product. Further, cosmetic manufacturers require accurate determination of the ingredients in cosmetics for formula analysis. Therefore, a method for the simultaneous determination of six polyhydroxyl compounds, Pro-Xylane, xylitol, sorbitol, mannitol, sucrose, and inositol, in cosmetics and toothpaste was established. According to this method, approximately 0.5 g of the sample was weighed into a 25 mL centrifuge tube. Water-dispersed and oil-in-water cosmetic samples were extracted using 10 mL water, followed by washing with 5 mL <i>n</i>-hexane and 5 mL ethyl acetate. The water-in-oil cosmetic samples were predispersed in 5 mL ethyl acetate, extracted using 10 mL water, and washed with 5 mL <i>n</i>-hexane. After filtration through a 0.22 μm membrane, the extracted solution was subjected to separation using an Ultimate XB-NH₂ column (250 mm×4.6 mm, 5 μm), employing gradient elution with acetonitrile and distilled water as the mobile phases. This was followed by detection using evaporative light-scattering detector (ELSD) and quantification using the external standard method. Optimization experiments were conducted to select chromatographic columns, extraction processes, and chromatographic conditions. Specifically, the Ultimate XB-NH₂ column and Ultimate XB-C₁₈ column were compared in terms of separation efficiency. Based on the separation efficiency and analysis time, the XB-NH₂ column was found to be more suitable as the separation column for this method. The effects of trichloromethane (TCM), ethyl acetate (EA), and <i>n</i>-hexane as predispersants and washing solutions were compared. Among them, the combination of ethyl acetate and <i>n</i>-hexane was found to be more suitable owing to its effective pre-dispersion capability and ability to remove both polar and nonpolar compounds from the extraction solution. The instrumental conditions were optimized using the gradient elution mode with acetonitrile and water as the mobile phase. The column temperature was set at 20 ℃, while the drift tube temperature and atomized gas pressure were set to 60 ℃ and 0.17 MPa, respectively. Under the optimized conditions, the method was validated in terms of linearity, sensitivity, recovery, and repeatability. The results showed that the six polyhydroxyl compounds exhibited excellent linearities within the range of 0.2-5.0 g/L, with correlation coefficients in the range of 0.991-0.996. Sensitivity is expressed as the limits of detection (LODs, <i>S/N</i>=3) and quantification (LOQs, <i>S/N</i>=10). The LODs and LOQs were 0.10% and 0.35%, respectively. Recovery tests were conducted at three levels (low, medium, and high) for oil-in-water cosmetics, wat","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"269-274"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883529/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569307","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Development of an ideological and political education design based on course characteristics: taking high performance liquid chromatography as an example].","authors":"Hui-Li Yang, Gang-Feng Tang, Jie Lei","doi":"10.3724/SP.J.1123.2024.04008","DOIUrl":"10.3724/SP.J.1123.2024.04008","url":null,"abstract":"<p><p>In response to the problems of the easy repetition of ideological and political education cases and the difficulty of evaluating ideological and political education, this study takes the classic experimental method of high performance liquid chromatography as an example to carry out the teaching practice of ideological and political education based on the characteristics of the course. First, the aim of the experiment, that is, the determination of preservatives and sweeteners in food, was introduced. Next, the specific practice processes, including case significance, case introduction, case implementation, case expansion, and effectiveness assessment, of two types of ideological and political programs, namely, universal and specialized cases, were introduced. Universal cases consider the importance of instrumental analytical experiments, while specialized cases consider the localization of high performance liquid chromatographs. We adjusted the ideological and political content of the instrumental analytical experimental course according to the course progress and actual experience of students, and integrated ideological and political education into the curriculum in stages. In addition to the functions of value guidance and ideological education, the role of ideological and political programs in promoting professional knowledge learning and innovation ability training was strengthened. We recommend that the effectiveness of ideological and political education be evaluated by mastering professional knowledge and improving innovative abilities.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"283-288"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883533/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569256","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Comprehensive instrumental analysis experiment: determination of gallium using inductively coupled plasma mass spectrometry].","authors":"Hai-Jiao Zheng, Ya-Ming Zhao, Xiao-Feng Wu, Hai Xu, Qiong Jia","doi":"10.3724/SP.J.1123.2024.04025","DOIUrl":"10.3724/SP.J.1123.2024.04025","url":null,"abstract":"<p><p>\"Admiring the lofty mountains, one realizes their own lack of talent.\" To further promote the implementation of new curriculum standards, a comprehensive instrumental analysis experiment was designed. Metabolomics, an emerging technology developed after genomics and proteomics, is an important part of systems biology. This study aims to explore the applications of metabolomics in the fields of environment and health. Sample pretreatment technology and detection methods for separating and enriching gallium were chosen through a literature review and group discussion. Students then experimentally analyzed the changes in metabolite content in cells cultured with metal-anticancer gallium drugs, which helped them understand the widespread application of metabolomics in the fields of environment and health. Additionally, material characterization was conducted using X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TG), and the gallium metal in metabolites was qualitatively and quantitatively analyzed using inductively coupled plasma mass spectrometry (ICP-MS). During discussions of this experiment, the teacher guided students in using large-scale instruments to solve problems comprehensively, fostering a research-based teaching approach to build a solid foundation for conducting efficient instrument analysis and comprehensive experiments within the classroom in future.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 3","pages":"289-294"},"PeriodicalIF":0.0,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11883518/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143569182","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Analysis of phthalate esters and their novel alternatives in indoor dust using comprehensive two-dimensional gas chromatography-time of flight mass spectrometry].","authors":"Lin-Xiao Wang, Ke Gao, Jian-Jia Li, Jia-Hui Peng, Zi-Yan Yang, Er-Ken Ya, Cong-Yi Zheng, Wei Wei, Li-Ping Lu, Shui-Yuan Cheng","doi":"10.3724/SP.J.1123.2023.12002","DOIUrl":"10.3724/SP.J.1123.2023.12002","url":null,"abstract":"&lt;p&gt;&lt;p&gt;A comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOF-MS) method was developed to analyze 25 traditional phthalate esters (PAEs) and 19 novel alternatives in indoor dust samples. PAEs are ubiquitous in indoor environments because they are widely used as plasticizers in a variety of consumer products, and potential health concerns have prompted the need for effective monitoring methods. In this study, dust samples were collected from various indoor settings in a university campus, including classrooms, cafeterias, laboratories, and dormitories, and were subsequently ultrasonically extracted with hexane-dichloromethane (1∶1, v/v) solution for 30 min. This method was chosen to maximize PAE recovery while minimizing potential interference from other compounds present in the dust matrix. Compounds were separated on a Rix-5MS column (30 m×0.25 mm×0.25 μm) as the first dimension, with a Rix-17Sil column (1.39 m×0.25 mm×0.25 μm) serving as the second dimension. The following temperature program was used: 60 ℃ for 1 min, then increasing to 220 ℃ at 20 ℃/min, followed by a further increase to 290 ℃ at 5 ℃/min, with the final temperature held for 8 min; this program was optimized to afford maximum target-compound resolution and sensitivity. The developed method rapidly, accurately, and sensitively detected the target PAEs and their alternatives under the optimal conditions, which included a carrier-gas flow rate of 1.4 mL/min, a modulation period of 4 s, and an injection-port temperature of 250 ℃. The 44 target compounds exhibited highly linear calibration curves across a content range of 1-500 μg/g, with all correlation coefficients exceeding 0.99. The limits of detection (LODs) of the method were determined to lie between 0.57 and 13.0 ng/g, which reflects the high sensitivity of the developed approach. At spiked levels of 1, 10, and 50 μg/g, the recoveries of the analyzed compounds varied from 72.8% to 125%, with relative standard deviations ranging from 1.29% to 14.8% (&lt;i&gt;n&lt;/i&gt;=3), which indicates that the method is highly precise and reliable. The developed method was used to analyze PAEs and their alternatives in 40 indoor dust samples, which revealed total contents of between 2.07 and 354 μg/g in dust samples. Di-2-ethylhexyl phthalate (DEHP) emerged as the most frequently detected compound, with contents ranging from \"not detected\" (nd) to 158 μg/g. The novel alternative, bis(2-ethylhexy) terephthalate (DEHTH), was also detected, with levels ranging from nd to 117 μg/g. Notably, significant differences in the compositions and contents of the PAEs and their alternatives were observed across various indoor environments, which suggests that diverse sources and exposure pathways exist for these compounds, highlighting the necessity for ongoing PAE monitoring and risk assessment in various indoor settings. In conclusion, the developed GC×GC-TOF-MS method provides a powerful tool for comprehensively analyzing","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 2","pages":"185-196"},"PeriodicalIF":0.0,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11755752/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143026279","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of glufosinate, glyphosate and their metabolites in sediment by ultra-high performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction].","authors":"Xiao Yang, Zhong-Gui Xie, Xiao-Ling Li, Wen-Wen Suo, Xiang-Yi Chen, Yi-Wen Wan","doi":"10.3724/SP.J.1123.2024.03008","DOIUrl":"10.3724/SP.J.1123.2024.03008","url":null,"abstract":"<p><p>Glufosinate (GLUF) and glyphosate (GLY) are nonselective phosphorus-containing amino acid herbicides that are widely used in agricultural gardens and noncultivated areas. These herbicides give rise to a number of key metabolites, with 3-methyl phosphinicopropionic acid (MPPA), <i>N</i>-acetyl glufosinate (<i>N</i>-acetyl GLUF), aminomethyl phosphonic acid (AMPA), <i>N</i>-acetyl aminomethyl phosphonic acid (<i>N</i>-acetyl AMPA), <i>N</i>-acetyl glyphosate (<i>N</i>-acetyl GLY), <i>N</i>-methyl glyphosate (<i>N</i>-methyl GLY) as the major metabolites obtained from GLUF and GLY. Extensive use of these herbicides may lead to their increased presence in the environment, especially aquatic ecosystems. An increasing number of research studies into the toxicities of GLUF, GLY, and their metabolites have shown that these herbicides are potentially toxic to aquatic biota. GLUF and GLY, as well as their metabolites, are extremely polar and water-soluble, and they lack chromogenic and fluorescent groups; therefore, their concentrations are difficult to determine using conventional methods. Most analytical methods used to date have largely depended on derivatization procedures, leading to overall determination processes that are tedious and time-consuming. Therefore, establishing a quick and sensitive method that does not require derivatives for determining GLUF, GLY, and their metabolites in water environments, including surface water, sediments, and aquatic organisms, is an important endeavor. In this study, a new approach was developed based on pass-through solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) to determine GLUF, GLY, and their metabolites, including MPPA, <i>N</i>-acetyl GLUF, AMPA, <i>N</i>-acetyl AMPA, <i>N</i>-acetyl GLY, and <i>N</i>-methyl GLY, in sediments. Samples were extracted with 4% (v/v) ammonia water and purified using PRiME HLB pass-through solid-phase extraction columns. The extracts were filtered through a polyethersulfone microfiltration membrane and analyzed by UHPLC-MS/MS. Compounds were separated on a Metrosep A Supp 5 column (150 mm×4.0 mm, 5 μm) using gradient elution with water and 200 mmol/L ammonium hydrogen carbonate solution containing 0.05% (v/v) ammonia water as the mobile phases. Analytes were detected using MS/MS with a negative electrospray ionization (ESI^-) source in the multiple reaction monitoring (MRM) mode. A matrix-matched external-standard approach was used for quantitative analysis. GLUF, GLY, and their metabolites were detected within 15 min with good peak shapes and high responses. Calibration curves were linear in the range of 2.0-200 μg/L, with correlation coefficients exceeding 0.995. This method delivered limits of detection (LODs) and limits of quantification (LOQs) of 5 μg/kg and 20 μg/kg, respectively, for GLUF, MPPA, <i>N</i>-acetyl-GLUF, <i>N</i>-acetyl AMPA, <i>N</i>-acetyl GLY, and <i>N</i>-methyl GLY, ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 2","pages":"155-163"},"PeriodicalIF":0.0,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11758234/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143026282","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Research advance of solid-phase microextraction based on covalent organic framework materials].","authors":"Ying-Chao Cheng, Yi-Yang Gao, Xiao-Min Li, Lu-Yu Chen, Fang DU, Jie Guo, Yi-Tong Meng, Min Sun, Juan-Juan Feng","doi":"10.3724/SP.J.1123.2024.01002","DOIUrl":"10.3724/SP.J.1123.2024.01002","url":null,"abstract":"<p><p>Solid-phase microextraction (SPME) is a fast and simple sample preparation technique that enables the enrichment of analytes, and it is used in combination with other detection techniques to provide accurate and sensitive analytical methods. SPME is widely used in environmental monitoring, food safety, life analysis, biomedicine, and other applications. The extractive coating is the core of the SPME technique, and the properties of the extractive coating greatly influence extraction selectivity and efficiency, as well as the enrichment effect. Therefore, the development of new and efficient extractive coating materials remains a hot topic in the analytical chemistry and sample preparation fields. Covalent organic frameworks (COFs) are a kind of porous crystalline network polymer materials formed by covalent bonds. Owing to the advantages of large specific surface area, high porosity, good stability, high designability, simple synthesis and post-modification, etc., it has been widely used in gas adsorption, catalysis, sensing and drug delivery. In recent years, COFs have attracted much attention in the field of sample preparation. A variety of novel COF-based SPME materials had been developed for extracting and enriching various types of analytes through <i>π</i>-<i>π</i> interaction, hydrophilic/hydrophobic interaction, electrostatic adsorption, and hydrogen-bonding, as well as pore effects. In this paper, the research advances of COFs for using in fiber-, in tube-, and membrane-based SPME over the past three years were discussed. Fiber surfaces had been modified with functionalized COFs or COF-hybrid materials for use in SPME through physical coating, in-situ growth, and chemical-bonding approaches. The combination of SPME fiber and chromatographic analysis can be used to detect a variety of analytes such as polycyclic aromatic hydrocarbons, phthalates, polychlorinated biphenyls, and pesticides in environmental and food samples, with good enrichment effects, wide linear ranges, and high sensitivity. Based on in tube-SPME, COFs-based monolithic column and fiber-filled tube as the extraction tubes were combined with high performance liquid chromatography online to develop highly sensitive detection methods for synthetic phenolic antioxidants and bisphenol compounds, respectively. In addition, COFs had also been used in membrane SPME technique, showing high efficiency in the extraction of trace polychlorinated biphenyls in environmental water. Finally, the development trends of COFs in the field of SPME was prospected.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 2","pages":"120-130"},"PeriodicalIF":0.0,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11758237/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143026276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of three metabolites of thromboxane A₂ and 8-iso-prostaglandin F_2α in urine by ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Si-Jia Liu, Fu-Rong Zhao, Ya-Lian Zhang, Xiao-Yu Sun, Meng-Meng Zhang, Kun Hou, Yun-Feng Cao","doi":"10.3724/SP.J.1123.2024.02004","DOIUrl":"10.3724/SP.J.1123.2024.02004","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Thromboxane A&lt;sub&gt;2&lt;/sub&gt; (TXA&lt;sub&gt;2&lt;/sub&gt;), a prothrombotic factor that induces platelet aggregation and thrombosis, acts as a vasoconstrictor by activating TXA&lt;sub&gt;2&lt;/sub&gt; receptors (TP receptors). TXA&lt;sub&gt;2&lt;/sub&gt; is extremely unstable and metabolizes into three major metabolites: 2,3-dinor thromboxane B&lt;sub&gt;2&lt;/sub&gt; (2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt;), 11-dehydro TXB&lt;sub&gt;2&lt;/sub&gt;(11-dh-TXB&lt;sub&gt;2&lt;/sub&gt;), and 11-dehydro-2,3-dinor TXB&lt;sub&gt;2&lt;/sub&gt;(11-dh-2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt;). 8-Iso-prostaglandin F&lt;sub&gt;2α&lt;/sub&gt;(8-iso-PGF&lt;sub&gt;2α&lt;/sub&gt;), a prostaglandin-like compound widely considered the best biomarker of oxidative stress, can also activate TP receptors. The accurate quantification of TXA&lt;sub&gt;2&lt;/sub&gt; metabolites and 8-iso-PGF&lt;sub&gt;2α&lt;/sub&gt; is critical in cardiovascular disease (CVD). In this study, a method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt;,11-dh-2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt;, 11-dh-TXB&lt;sub&gt;2&lt;/sub&gt;, and 8-iso-PGF&lt;sub&gt;2α&lt;/sub&gt; in human urine. Urine samples were collected from healthy volunteers and patients with CT- or MRI-confirmed ischemic stroke occurring less than 48 h earlier, and cryopreserved at -80 ℃ within 1 h after collection. The urine samples were thawed at room temperature and acidified to pH 2.0-4.0 using hydrochloric acid. The supernatant was collected after centrifugation. A total of 1 mL of each urine sample was added with 100 μL of the internal standard working solution and mixed well. The samples were loaded onto a C18 SPE column (50 mg). The SPE cartridges were preconditioned with 500 μL of methanol and then equilibrated with 500 μL of water. After sample loading, the SPE cartridges were washed with 500 μL of water, 500 μL of 5% methanol aqueous solution containing 0.5% (v/v) ammonia, and 500 μL of 5% methanol aqueous solution containing 2% (v/v) formic acid. The cartridges were dried, and the analytes were eluted with 400 μL of methanol. The eluents were dried and subsequently reconstituted with 50 μL of 13% acetonitrile aqueous solution. After filtration through a filter membrane, the samples were analyzed on an ACQUITY UPLC&lt;sup&gt;®&lt;/sup&gt; BEH phenyl column (50 mm×2.1 mm, 1.7 μm) via gradient elution using 2 mmol/L ammonium acetate aqueous solution containing 0.002% (v/v) ammonia and acetonitrile as the mobile phases. The flow rate was 0.3 mL/min, and the column temperature was 40 ℃. The analytes were determined in negative electrospray ionization and multiple-reaction monitoring modes. The four target compounds showed satisfactory linearity within the relevant ranges, with linear correlation coefficients (&lt;i&gt;R&lt;/i&gt;&lt;sup&gt;2&lt;/sup&gt;) greater than 0.99. The limits of detection of the method were 0.02 ng/mL for 2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt; and 0.01 ng/mL for 11-dh-2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt;, 11-dh-TXB&lt;sub&gt;2&lt;/sub&gt;, and 8-iso-PGF&lt;sub&gt;2α&lt;/sub&gt;. The limits of quantification were 0.1 ng/mL for 2,3-dinor-TXB&lt;sub&gt;2&lt;/sub&gt; and ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 2","pages":"148-154"},"PeriodicalIF":0.0,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11755747/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143026283","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}