Se pu = Chinese journal of chromatography最新文献

{"title":"[Determination of trace polychlorinated biphenyls in environmental water samples by solid-phase microextraction-gas chromatography-tandem mass spectrometry using carbon nanotube composite microspheres materials].","authors":"Xin-Li Song, Shu-Qi Zhu, Yu-Xin Wu, Li-Yan Zhong, Yu-Qing Liu","doi":"10.3724/SP.J.1123.2025.01004","DOIUrl":"10.3724/SP.J.1123.2025.01004","url":null,"abstract":"<p><p>Polychlorinated biphenyls （PCBs） pose serious threats to the environment and human health because they are among the most common and persistent organic pollutants globally. In this study， six PCBs were extracted from environmental water samples using multiwalled carbon nanotubes （MWCNTs） on polystyrene （PS） microspheres as the solid-phase microextraction （SPME） coating material for gas chromatography-tandem mass spectrometry （GC-MS/MS）. This coating material is highly stable and exhibited a high extraction efficiency. 2，2'，5，5'-Tetrachlorobiphenyl （PCB-52）， 2，2'，4，5，5'-pentachlorobiphenyl （PCB-101）， 2，3'，4， 4'，5-pentachlorobiphenyl （PCB-118）， 2，2'，3，4，4'，5'-hexachlorobiphenyl （PCB-138）， 2，2'，4，4'，5，5'-hexachlorobiphenyl （PCB-153） and 2，2'，3，4，4'，5，5'-heptachlorobiphenyl （PCB-180） were chosen as target analytes. The main extraction factors were optimized using a single-factor optimization method， which led to the following optimum extraction conditions： adsorption time， 50 min； agitation speed， 600 r/min； pH， 6； NaCl concentration， 1.5 mol/L； desorption temperature， 280 °C； and desorption time， 4 min. GC coupled with triple quadrupole mass spectrometry was used to quantify PCBs in water samples. The chromatographic separation system was equipped with a TG-5 SILMS column （30 m×0.25 mm×0.25 μm）， with electron impact ionization and multi-reaction monitoring modes used during mass spectrometry. Five batches of MWCNT@PS were used as SPME coating materials， which were determined to have relative standard deviations （RSD） of less than 8.8% for the six PCBs. The reusability of the MWCNT@PS coating was also investigated； RSD of the recoveries of 2.8%-9.3% were obtained after ten SPME cycles with the same coating. These results reveal that the MWCNT@PS coating materials are highly stable and reusable in SPME applications， with good results obtained under the optimal conditions. The established method exhibited linearity in the range of 0.03-1 000 ng/L for PCB-52 and PCB101， 0.07-1 000 ng/L for PCB118， PCB138， and PCB 153， and 0.10-1 000 ng/L for PCB-180， with correlation coefficients of 0.993-0.998. Limits of detection and quantification （LODs and LOQs， respectively） of 0.01-0.03 and 0.03-0.10 ng/L were determined for the developed method. The intra- and inter-day precisions exhibited RSDs of 1.64%-8.16% and 2.83%-8.41%， respectively， at 2 ng/L， 3.31%-7.19% and 3.79%-9.12%， respectively， at 10 ng/L， and 2.70%-9.38% and 4.04%-8.56%， respectively， at 100 ng/L. The established method was used to determine six PCBs in barreled drinking water， rainwater， and three environmental river water samples. No PCBs were found in barreled drinking water， rain water and river water. Satisfactory recoveries of 82.4%-113.2% were achieved at low， medium， and high levels. Accordingly， the MWCNT@PS-composite-coating-material-based SPME-GC-MS/MS method is accurate and effective. This study revealed that MWCNT@PS composites provide a good avenue for the rapid and sensitive ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 10","pages":"1154-1161"},"PeriodicalIF":0.0,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12481668/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145133158","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 identification and detection of four novel isoxazoline drugs in bovine-origin foods using ultra-high performance liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry].","authors":"Cheng Yang, Wei-Xia Zhu, Ya-Feng Liu, Wei Wei, Fang Zhao, Kai Hu, Wen-Jie Zhao","doi":"10.3724/SP.J.1123.2024.11012","DOIUrl":"10.3724/SP.J.1123.2024.11012","url":null,"abstract":"<p><p>Isoxazoline drugs （ISOs） are a class of five-membered heterocyclic compounds containing N and O atoms. They can inhibit <i>γ</i>-aminobutyric acid gated chloride channels and are widely used in the treatment of parasitic diseases in poultry. The intake of animal-derived foods by humans is an important way to come into contact with ISOs. Excessive use of ISOs can lead to their residues in animal-derived foods， thereby threatening human health and causing neurotoxicity and hepatotoxicity. To address the safety issues caused by ISO residues in animal-derived foods， an ultra-high performance liquid chromatography-quadrupole/linear ion trap mass spectrometry （UHPLC-Q/Trap MS） analytical method for four novel ISOs （fluralaner， sarolaner， afoxolaner， lotilaner） in bovine-origin foods （including milk， beef and bovine liver） was established. The sample was first extracted with acetonitrile and then purified with PRiME HLB solid phase extraction （SPE） column. Using 5 mmol/L ammonium acetate aqueous solution and acetonitrile as the mobile phase， after separation by Shim-pack GIST C18-AQ （100 mm×2.1 mm， 2.7 μm） chromatography column， the analysis was carried out in the multi-reaction monitoring （MRM） mode by information-dependent acquisition （IDA）， enhanced product ion scanning （EPI） and spectral library retrieval， and quantification was performed using the external standard method. The results showed that the four ISOs had good linear relationships within their respective mass concentration ranges. The correlation coefficients （<i>r</i>） were all ≥0.993 6， and the limits of detection （LODs） and quantification （LOQs） were 0.2-0.5 μg/kg and 0.5-1.0 μg/kg， respectively. Under the low， medium and high spiked levels （1， 2 and 10 μg/kg）， the recoveries of the four ISOs ranged from 67.6% to 118.9%， and the relative standard deviations （RSDs） ranged from 2.0% to 20.0%. In addition， in this study， qualitative screening and analysis of the target compounds were conducted through MRM-IDA-EPI combined with spectral library retrieval. Dual qualitative analysis of the target compounds was carried out based on information such as retention time and EPI fragment ions， which improved the accuracy of qualitative analysis and effectively eliminated the interference of false positive results. This method features low LODs and good recoveries. It is also simple and rapid to operate， with high sensitivity and accuracy. It can achieve qualitative and quantitative analysis of new ISOs residues in bovine-origin foods. This study can provide technical support for food safety agencies to implement preventive measures against new ISOs in animal foods.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1045-1052"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412015/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002435","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 <i>N</i>-（1，3-dimethylbutyl）-<i>N'</i>-phenyl-<i>p</i>-phenylenediamine-quinone in urine and dust by ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Zhu-Liang-Zi Lu, Fen-Fang Deng, Zhi-Jun Bai, Rong-Fei Peng, Lei Tan","doi":"10.3724/SP.J.1123.2025.02010","DOIUrl":"10.3724/SP.J.1123.2025.02010","url":null,"abstract":"<p><p>An ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was established to determine <i>N</i>-（1，3-dimethylbutyl）-<i>N'</i>-phenyl-<i>p</i>-phenylenediamine-quinone （6PPD-Q） in human urine and dust in order to understand the internal and external exposure levels in humans. The sample preparation conditions were systematically investigated and the chromatographic conditions and MS parameters were optimized. Briefly， internal standard ¹³C₆-6PPD-Q （0.1 ng） was added to a urine sample. Glutathione and NaCl were added after equilibration for 30 min. The mixture was then twice ultrasonically extracted with ethyl acetate. Internal standard ¹³C₆-6PPD-Q （1.0 ng） was also added to a dust sample and the mixture was twice ultrasonically extracted with <i>n</i>-hexane. The combined organic phases were concentrated to near-dryness and then redissolved for instrumental determination， which was performed on a Phenomenex Kinetex F5 column （100 mm×3 mm， 2.6 μm）， with the target analyte gradient eluted using 10 mmol/L ammonium acetate aqueous solution containing 0.01% formic acid and acetonitrile. Positive electrospray ionization （ESI⁺） and multiple reaction monitoring （MRM） modes were used for identification purposes， and an isotope-labeled internal standard was added for quantification. Good linearities were achieved under the optimized conditions within the 0.01-4.00 and 0.01-20.0 μg/L ranges for urine and dust， respectively， with correlation coefficients of 0.999 9 and 0.999 3， respectively. Limits of detection （LODs） were 0.6 ng/L （urine） and 0.018 ng/g （dust）. Spiked recoveries of 6PPD-Q were 90.3%-94.1% at low， medium， and high spiked levels， with intra-day and inter-day precisions of 0.9%-5.9% and 1.1%-6.3%， respectively. Matrix-effect investigations revealed that 6PPD-Q exhibited weak matrix effects in urine and dust after correction with the isotopic internal standard. The developed method was used to analyze 120 human urine samples， which led to a 6PPD-Q detection frequency of 74.2%， with mass concentrations ranging from <LOD to 13 ng/L， with average and median mass concentrations of 2 and 1 ng/L， respectively. However， 6PPD-Q was detected with a frequency of 100% in 31 indoor dust samples with contents of 1.8-24.9 ng/g， and average and median contents of 5.23 -3.05 ng/g， respectively. The developed method is accurate， reliable， highly sensitive， and it is suitable for the rapid determination of 6PPD-Q in human urine and dust samples.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1025-1033"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412019/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002408","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":"[A protein-specific quantitative detection method based on polyacrylamide gel electrophoresis and online fluorescence imaging].","authors":"Rui Zou, Zi-Xian Yu, Ze-Hua Guo, Hao-Zheng Dai, Qiang Zhang, Wei-Wen Liu, Cheng-Xi Cao","doi":"10.3724/SP.J.1123.2024.12017","DOIUrl":"10.3724/SP.J.1123.2024.12017","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Specific protein detection plays a crucial role in biological analysis and clinical diagnostics， serving as an essential tool for disease diagnosis， therapeutic monitoring， and biological research. However， conventional methods such as immunofixation electrophoresis （IFE） and western blotting （WB） suffer from complex workflows， time-consuming operations， and limited quantification capabilities owing to intricate staining and de-staining procedures. In addition， these traditional immunological detection methods require extensive manual handling and specialized expertise， while low levels of automation restrict their applicability to high-throughput or large-scale analysis scenarios. Moreover， the multistep nature of these methods increases the risk of experimental errors and compromises quantification accuracy.Herein， we present a quantitative protein immune polyacrylamide gel electrophoresis （PAGE） detection method that combines immune-recognition principles with online fluorescence imaging technology， thereby offering a rapid and specific approach for quantifying target proteins. The developed method exploits the specificity of fluorescently labeled antibodies and the separation capability of PAGE， with formaldehyde crosslinking used to stabilize antigen-antibody complexes under the denaturing conditions of electrophoresis， thereby ensuring reliable quantification. The entire experimental workflow can be completed within 1.5 h and consists of three main steps. Firstly， the target protein is incubated with fluorescently labeled antibodies at room temperature for 0.5 h to form immune complexes， after which they are crosslinked using formaldehyde. The cross-linked samples are then loaded onto polyacrylamide gels and separated under optimized electrophoresis conditions （120 V， 15 min； 150 V， 15 min； 200 V， 15 min）. Electrophoretic separation is finally monitored in real-time using an online fluorescence imaging system， which enables direct visualization of protein migration and eliminates the need for post-separation processing. Three distinct bands are observed on the precast gel following immune PAGE separation： the immune complexes at the uppermost position， the free fluorescent antibodies in the middle， and other proteins at the bottom. ImageJ software is used to analyze the electrophoresis pattern， and quantification is achieved based on the linear relationship between the fluorescence intensity of the free antibody and the mass concentration of the target protein. We systematically validated the performance of the method using human transferrin （TRF） as the model antigen protein and fluorescein-isothiocyanate-labeled （FITC-labeled） anti-TRF IgG antibody （anti-TRF IgG-FITC） as the detection probe， which involved analyzing three key aspects： the necessity of the formaldehyde-crosslinking step for maintaining immune complex stability， antibody recognition specificity in complex samples， and the linear correlation between the fluorescence si","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1070-1077"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412021/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002468","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 79 pesticide residues in fruits and vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Le Zhao, Xian-Jun Liu, Hao Zhang, Jian Li, Liang Cai, Xiang Fan, Tan-Yao Li, Dong-Yang Chen","doi":"10.3724/SP.J.1123.2025.02015","DOIUrl":"10.3724/SP.J.1123.2025.02015","url":null,"abstract":"<p><p>Pesticide residues in fruits and vegetables are becoming a serious issue. These residues can affect the quality of agricultural products and people's health. Therefore， it has become crucial to effectively monitor and control pesticide residues in the food safety field. In this study， a rapid and effective QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry （QuEChERS-UPLC-MS/MS） method was established for the simultaneous determination of 79 typical pesticides in vegetables and fruits， including organophosphates， carbamates， and pyrethroids. The pretreatment， UPLC， and MS/MS conditions were optimized. The fruit and vegetable samples were extracted with frozen acetonitrile after pulverization and homogenization， cleaned up by the QuEChERS method， filtered through a centrifugal membrane， and analyzed by UPLC-MS/MS. The separation was carried out on an ACQUITY UPLC HSS T3 column （100 mm×2.1 mm， 1.8 μm） with gradient elution. The aqueous and organic phases were water-methanol （98∶2， v/v） and methanol-water （98∶2， v/v） respectively， both with 5 mmol/L ammonium acetate and 0.1% formic acid. A triple quadrupole mass spectrometer was used in positive-ion electrospray ionization （ESI⁺） scanning mode， with target pesticide residues quantified using the matrix-matched standard-curve method. The results showed that under the optimized conditions， the 79 target compounds were determined with good linearities in the range of 0.1-200 μg/L， and the correlation coefficients （<i>r</i>） were all greater than 0.990. The limits of detection （LODs） and limits of quantification （LOQs） of the 79 compounds were in the range of 0.01-4.0 μg/kg and 0.03-13.0 μg/kg. The recoveries at three spiked levels ranged from 78.2% to 119.8%， with relative standard deviations （RSDs） all less than 15.8%. The established method was successfully applied to 80 samples of fruits and vegetables from Hunan province. As a result， 19 pesticides were detected in 31 samples， and thiamethoxam， acetamiprid and clothianidin being the most highly detected with a content range of 0.012-2.62 mg/kg； According to the data of the Hunan province survey yearbook， the percentages of acceptable daily intake （%ADI） for chronic dietary exposure of the detected neonicotinoid insecticides （thiamethoxam and clothianidin） have been calculated. The results indicate that the %ADI of clothianidin in fruits and vegetables ranged from 5.74% to 0.36%， respectively， and the %ADI of thiamethoxam in fruits and vegetables ranged from 0.40% to 19.50%. The %ADI of both pesticides were found to be less than 100%， indicating they are within acceptable limits. The method is simple， sensitive， accurate， and suitable for the simultaneous determination of multiple pesticide residues in fruits and vegetables.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1053-1062"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412020/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002399","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 26 perfluorinated and polyfluoroalkyl compounds in human serum by solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry].","authors":"Ying-Xiao Yue, Ya-Ting Bian, Yu-Fan Cheng, Lu He, Dan Wang, Pei-Xia Yan, Wei Yan, Gui-Ying Liu, Huan Song, Liang-Po Liu","doi":"10.3724/SP.J.1123.2024.10002","DOIUrl":"10.3724/SP.J.1123.2024.10002","url":null,"abstract":"<p><p>Perfluorinated and polyfluoroalkyl compounds （PFASs） represent a category of synthetic chemicals renowned for their environmental persistence. Owing to their hydrophobic， oleophobic， and high-temperature-resistant properties， PFASs are extensively utilized in industrial， agricultural， and civilian sectors， including applications in leather， textiles， flame-retardant materials， lubricants， and coatings， among others. PFASs can accumulate within the human body， exhibiting multi-organ toxicity. Continuous monitoring of PFASs with ambiguous toxicity profiles is vital for evaluating human exposure and associated health risks. Consequently， the establishment of a high-throughput and highly sensitive detection method is of paramount importance for accurately assessing the exposure levels of PFASs in the human body. In this study， a commercial high-throughput HMR-Lipid 96-well solid-phase extraction plate was adopted， combined with high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）， to establish a simple， efficient method that can simultaneously quantitatively detect 26 PFASs in human serum. Serum samples were extracted using the HMR-lipid 96-well solid-phase extraction plate. The Phenomenex C₁₈ chromatography column （250 mm×4.6 mm， 5 μm） was used as the capture column and connected between the liquid chromatography mixer and the autosampler to avoid high background pollution. The target compounds were separated by the Accucore C₁₈ chromatography column （100 mm×2.4 mm， 2.6 μm） and analyzed using the electrospray ionization with negative ion scanning mode and multiple reaction monitoring （MRM） mode. The methodological validation results indicated that the 26 PFASs had good linear relationships within the range of 0.2-100 ng/mL， with correlation coefficients （<i>r</i>） of 0.995 1-0.999 9. The limits of detection （LODs） and quantification （LOQs） were 0.01-0.15 ng/mL and 0.02-0.47 ng/mL， respectively. At three spiked levels of low， medium and high， the recoveries of the 26 PFASs ranged from 80.1% to 119.5%， and the relative standard deviations （RSDs） ranged from 0.5% to 11.9%. This method has the advantages of high sensitivity， good accuracy， simple operation， fast extraction speed， low reagent consumption and small sample volume required. It is suitable for large-scale population biological monitoring and provides a scientific method support for accurately assessing the exposure of PFASs in the human body and its potential health risks.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1005-1013"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412018/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002482","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":"[A large-scale method for the enrichment and identification of N-glycopeptides in microscale plasma samples].","authors":"Xin-Yi Yang, Wei-Jie Qin","doi":"10.3724/SP.J.1123.2025.04004","DOIUrl":"10.3724/SP.J.1123.2025.04004","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Blood， which forms part of the systemic circulatory system， contains proteins from various tissues and organs. Hence， blood samples are ideal vehicles for studying diseases and physiological states. Plasma is an important component of blood and is essential for clinical proteomics research. Plasma contains rich physiological and pathological information； consequently， it is an ideal medium for discovering disease-related biomarkers. Protein N-glycosylation is a key post-translational modification route. This route is widely involved in biological processes such as intercellular communication， immune regulation， and signal transduction. Changes resulting from aberrant N-glycosylation are closely associated with various pathological conditions， including autoimmune and neurodegenerative diseases and tumors. Hence， N-glycosylation proteomics is highly valuable during biomarker and drug-target development. However， efficiently enriching N-glycopeptides in biological samples before detection by mass spectrometry （MS） is difficult. This is because the highly abundant unmodified peptides result in signal suppression. Consequently， achieving deep N-glycoproteomic coverage is a key challenge， particularly for trace plasma samples， for which in-depth studies are currently lacking. In this study， we developed a strategy for comprehensively profiling trace N-glycopeptides in plasma. This includes an efficient enrichment method in combination with highly sensitive MS. The developed approach integrates glycopeptide enrichment using advanced hydrophilic interaction liquid chromatography （HILIC） with state-of-the-art MS platforms. This significantly enhances detection depth and sensitivity during N-glycosylation analysis using minimal plasma volumes. Selectivity and efficiency during N-glycopeptide enrichment were maximized by systematically optimizing key HILIC-packed stationary-phase parameters. These parameters include chemical composition， pore size， and surface modification. Additionally， the elution gradient was fine-tuned to improve glycopeptide recovery. This optimization process delivered high N-glycopeptide specificity， even in complex plasma matrices. To overcome the limitations of single-platform MS， we implemented a complementary dual-platform strategy. This strategy combines the high-speed， high-resolution capabilities of the Tims TOF Pro 2 instrument with the ultra-high mass accuracy and resolution of the Orbitrap Lumos spectrometer. The former instrument facilitates the rapid and sensitive identification of glycopeptides， particularly for low-abundance species. It exploits the trapped ion mobility spectrometry （TIMS） and parallel accumulated sequential fragmentation （PASEF） technology. The Orbitrap Lumos provides exceptional mass accuracy and high-resolution MS/MS spectra that enable confident glycopeptide structural characterization. This synergistic approach significantly expands the N-glycopeptide identification depth and ensures compreh","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"996-1004"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412023/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002392","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":"[Advances in the development of analysis techniques for organophosphate diesters in water].","authors":"Jie Chen, Ming-Liang Liu, Lu Wu, Feng Xu, Jing Lyu, Lin-Hai Chen, Wei Li, Jie Fu, Jian-Jie Fu","doi":"10.3724/SP.J.1123.2025.02007","DOIUrl":"10.3724/SP.J.1123.2025.02007","url":null,"abstract":"<p><p>Organophosphate triesters （tri-OPEs） are synthetic phosphate derivatives that are primarily used as flame retardants and plasticizers. Tri-OPEs have become significant aquatic contaminants owing to their large production volumes and wide range of applications. Organophosphate diesters （di-OPEs） are closely related to tri-OPEs. Aside from emissions resulting from the production and usage of di-OPEs themselves， tri-OPEs can become transformed into di-OPEs， which also provides a significant source of this environmental contaminant. The physicochemical properties of a di-OPE depend significantly on its structure， which provides challenges for their detection and analysis， including low extraction efficiencies， chromatographic separation difficulties， and a lack of highly sensitive quantitative methods for their analysis. An increasing number of studies have found that di-OPEs are present in industrial/domestic wastewater， surface water， and drinking water， with some concentrations in surface water and tap water close to or even higher than those of the corresponding tri-OPEs. Additionally， certain di-OPEs are somewhat more toxic than the corresponding tri-OPEs； hence， awareness that di-OPEs are present in aquatic environments has raised widespread concern. This review first systematically outlines the physicochemical properties of common di-OPEs and their potential sources based on previous research into di-OPEs in water matrices. In addition， the use of solid phase extraction （SPE） technology to extract， enrich， and purify di-OPEs from water matrices is summarized， while the advantages and limitations of SPE methodologies are critically evaluated. Furthermore， the use and distinctive features of reverse-phase chromatography， ion-pair reverse-phase chromatography， and hydrophilic interaction liquid chromatography （HILIC） for the chromatographic separation of di-OPEs are comprehensively summarized and compared. At the same time， advances in the quantitative analysis of di-OPEs using liquid chromatography-tandem triple quadrupole mass spectrometry （LC-MS/MS） and liquid chromatography-high-resolution mass spectrometry （LC-HRMS） are reviewed. Finally， in terms of efficient collection of water samples and high-throughput pretreatment of di-OPEs in water matrices， the prospect of developing novel sampling and on-site enrichment technologies for new pollutants in water matrices based on the principle of dispersed solid phase extraction is proposed. Additionally， the prospect of using liquid chromatography tandem high-resolution mass spectrometry for high-throughput screening and high-sensitivity detection of di-OPEs and unknown transformation products of tri-OPEs has been proposed.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"987-995"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412014/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002394","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 bisphenol compounds in human urine by solid supported liquid-liquid extraction-ultra-high performance liquid chromatography-tandem mass spectrometry].","authors":"Yu'e Jin, Lan-Ge Zhang, Jing-Xian Zhou, Jin-Jing Ma, Li-Li Yuan, Ping Xiao, Guo-Quan Wang","doi":"10.3724/SP.J.1123.2024.11032","DOIUrl":"10.3724/SP.J.1123.2024.11032","url":null,"abstract":"<p><p>Bisphenol A （BPA） and its analogs are collectively termed bisphenol compounds （BPs）， which are predominantly utilized in the manufacturing of polycarbonate plastics and epoxy resins. BPs are ubiquitous in diverse environmental matrices， human tissues， and metabolic products. Extensive research has demonstrated that BPs exert adverse effects on the nervous， reproductive， immune， and metabolic systems. After exposure in humans， BPs are primarily excreted in urine. Consequently， the development of efficient and robust analytical methods for BPs quantification in urine is essential for assessing population exposure levels. In this study， solid supported liquid-liquid extraction （SLE） was combined with ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） technology to establish a high-throughput determination method for 17 BPs in human urine. After enzymatic hydrolysis treatment of the samples， the steps of fully automatic SLE purification， nitrogen blowing concentration and redissolution were carried out successively. Separation was performed using a CAPCELL PAK ADME chromatography column （100 mm×2.1 mm， 2 μm）， and gradient elution was carried out with 0.05 mmol/L ammonium fluoride aqueous solution and 0.05 mmol/L ammonium fluoride methanol solution as the mobile phases. MS detection was carried out using the electrospray ionization （ESI） negative ion scanning mode under the multi-reaction monitoring （MRM） mode. Qualitative analysis was conducted based on retention time and ion abundance ratio， and quantitative analysis was performed using the internal standard method. Under the optimized conditions， 17 BPs can be effectively separated. The linear relationships of the 17 BPs within the corresponding mass concentration ranges were good， and the correlation coefficients （<i>r</i>） were ≥0.998 6， the limits of detection （LODs） and quantification （LOQ） were 0.002-0.489 μg/L and 0.005-0.986 μg/L， respectively. Children's mixed urine samples with low background content were selected as the matrix， and then spiked recovery tests were conducted at three spiked levels （low， medium and high）. The results showed that the recoveries of 17 BPs were 61.1%-121.7%， the intra-day RSDs were 1.3%-11.2%， and the inter-day RSDs were 3.7%-19.0%. This method was used to determine 50 random urine samples， and the results showed that a total of 11 BPs were detected. Among them， bisphenol S （BPS） and BPA had the highest detection rates， which were 98.0% and 86.0% respectively， and the median detection levels were 0.075 μg/L and 0.829 μg/L respectively. This method is simple to operate， sensitive and reliable. It is suitable for the rapid quantitative analysis of 17 BPs in human urine and can provide effective technical support for the risk assessment of BPs exposure in the population.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1014-1024"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412013/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002413","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":"[Rapid determination of five antipyretic analgesics in surface water by online solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry].","authors":"Ping He, Li-Qun Wang, Shan Zhou, Bao-Feng Zhang, Xuan Jia, Yi Chi, Zhen-Qi Xu, Wei Tang","doi":"10.3724/SP.J.1123.2024.10018","DOIUrl":"10.3724/SP.J.1123.2024.10018","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Antipyretic analgesics are typical pharmaceutical and personal care products （PPCPs） that are widely used in our daily life because they relieve fever and pain， and have anti-inflammatory and anti-rheumatic properties. These drugs inhibit the synthesis and release of prostaglandins （PGs） in the neurons of the anterior hypothalamus and exert therapeutic effects as a consequence. However， these drugs are relatively commonly misused and abused， often owing to a lack of proper medication guidance. As a result， these drugs enter the environment via various pathways， including wastewater treatment plants， agricultural runoff， and improper disposal， thereby posing potential threats to human health and ecosystems. The presence of these contaminants in surface water has become an environmental safety concern that necessitates the development of rapid， accurate， and high-throughput analysis methods. In this study， an analytical method was established for the determination of five antipyretic analgesics （ibuprofen， aminophenazone， antipyrine， phenacetin， and naproxen）. The developed method is based on online solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry （online SPE-UHPLC-MS/MS）， which provides a high degree of automation and efficiency. Water samples were collected and filtered through 0.2-μm regenerated cellulose （RC） filter membranes， after which Na&lt;sub&gt;2&lt;/sub&gt;EDTA and an internal standard were added. An aliquot （0.9 mL） of each sample was injected into the online SPE system using an automatic sampler. Samples were first adsorbed on a PLRP-S online SPE column， washed with 0.05% formic acid aqueous solution， and finally gradient-eluted with a mobile phase composed of 0.2 mmol/L ammonium fluoride solution and methanol-acetonitrile （1∶1， v/v）. Analytes were separated on a ZORBAX Eclipse Plus C18 column， detected by multiple reaction monitoring with electrospray ionization in both positive- and negative-ion modes， and quantified using the internal-standard method.The five antipyretic analgesics were effectively separated under the optimized experimental conditions and showed good linearities within their respective concentration ranges， with correlation coefficients （&lt;i&gt;r&lt;/i&gt;） greater than 0.998. The method detection limits （MDLs） ranged from 0.05 to 0.20 ng/L， and the method quantification limits （MQLs） ranged from 0.20 to 0.80 ng/L. The five antipyretic analgesics exhibited average recoveries of between 64.2% and 112%， with relative standard deviations （RSDs， &lt;i&gt;n&lt;/i&gt;=6） of 2.06%-8.99% at low， medium， and high spiked levels. Furthermore， the method was successfully used to analyze water samples from the Hangzhou section of the Qiantang River， in which four target compounds were detected， with antipyrine found to have the highest mass concentration. This newly developed method features a high degree of automation， facilitates the injection of large volumes， and enables online enrichment， purif","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"43 9","pages":"1063-1069"},"PeriodicalIF":0.0,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12412016/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145002431","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}