Se pu = Chinese journal of chromatography最新文献

{"title":"[Occurrence characteristics， neurotoxicity risk， and potential mechanisms of traditional phthalate esters and novel alternatives in indoor dust].","authors":"Wei Li, Ke Gao, Kai Hua, Linxiao Wang, Wei Wei, Liping Lu","doi":"10.3724/SP.J.1123.2025.06025","DOIUrl":"10.3724/SP.J.1123.2025.06025","url":null,"abstract":"<p><p>Traditional phthalate esters （PAEs） and their novel alternatives are widely used as plasticizers. Owing to their non-covalent bonding with polymer matrices， these compounds readily migrate from materials and accumulate in indoor dust， posing potential risks to human health. Although their carcinogenic and reproductive toxicities have been extensively studied， their neurotoxicity， particularly that of novel alternatives， remains poorly understood. To address this knowledge gap， this study adopted an integrated approach combining pollution profiling， health risk assessment， and mechanistic investigation to systematically evaluate the neurotoxicity risks and potential mechanisms of PAEs and their alternatives in typical campus microenvironments （classrooms， laboratories， offices， cafeterias， and dormitories）. The contamination profile of target compounds in indoor dust was determined using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry （GC×GC-TOF MS）. By integrating three exposure pathways （ingestion， inhalation， and dermal contact of dust） with absorption， distribution， metabolism， excretion， and toxicity （ADMET） models， the estimated daily intakes （EDIs） and neurotoxic health risks for different populations were assessed. Furthermore， network toxicology and molecular docking techniques were employed to elucidate the potential toxic mechanisms. Results indicated that dormitories exhibited the highest contents of target compounds， with major components including di-2-ethylhexyl phthalate （DEHP）， di（2-ethylhexyl） tetrahydrophthalate （DEHTH）， acetyl tri-n-butyl citrate （ATBC）， and trioctyl trimellitate （TOTM）. Exposure assessment identified ingestion as the predominant exposure route. Using the ADMET model， toxicity equivalency factor （TEF） and toxic equivalent quantity （TEQ） were quantified for five neurotoxicity-related health endpoints， including phenotypic neurotoxicity， estrogen receptor activity， oxidative stress， mitochondrial dysfunction， and DNA damage. Risk assessment based on TEQ revealed that females aged 18-60 years faced higher neurotoxicity risks than males， although no statistically significant gender differences in EDI were observed across all age groups. Mechanistically， network toxicology identified 59 core targets associated with neurotoxicity， including oncogene， non-receptor tyrosine kinase （SRC）， serine/threonine kinase 1 （AKT1）， estrogen receptor 1 （ESR1）， mitogen-activated protein kinase （MAPK1， MAPK3）， heat shock protein 90 alpha family class a member 1 （HSP90AA1）， and Kirsten rat sarcoma viral oncogene homolog （KRAS）. Functional enrichment analysis showed that these core targets were predominantly enriched in pathways related to endocrine resistance and cancer， suggesting that these compounds may induce neurotoxicity by disrupting cellular homeostasis and signal transduction. Molecular docking supported specific binding interactions between representative compounds and co","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 5","pages":"575-588"},"PeriodicalIF":0.0,"publicationDate":"2026-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13150829/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147848514","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":"[Deep eutectic solvent and improved needle filter-based liquid-membrane microextraction combined with high performance liquid chromatography for the determination of sulfonamide and fluoroquinolone residues in milk].","authors":"Rui-Ming Xu, You-Yi Wu, Zhi-Hao Gu, Wei Wei, Xing-Yu Lu, Zi-Han Xia","doi":"10.3724/SP.J.1123.2025.03012","DOIUrl":"10.3724/SP.J.1123.2025.03012","url":null,"abstract":"<p><p>Antibiotic residues in dairy products pose serious threats to food safety and affect human health. To accurately determine the level of sulfonamide and fluoroquinolone residues in milk， a deep eutectic solvent and improved needle filter-based liquid membrane microextraction （DES&INF-LMME） method combined with high performance liquid chromatography （HPLC） was developed for their determination in this study. Octanoic acid （hydrogen bond donor） and thymol （hydrogen bond acceptor） were selected to synthesize hydrophobic deep eutectic solvent， which acted as supporting liquid membrane （SLM） and extractant in the LMME process. Further investigations were conducted to examine the effects of various factors on extraction efficiency， including type and volume of DES， molar ratio of thymol to octanoic acid， type of extraction membrane， sample volume， salt type and addition amount， pH value， stirring speed and extraction time. The optimal extraction conditions were determined as follows： DES∶thymol-octanoic acid=2∶1 （<i>n/n</i>）， 100 μL； filter membrane， polytetrafluoroethylene （PTFE）； sample volume and pH， 30 mL （addition of 3 g ammonium sulfate） and pH=7； stirring speed， 400 r/min； extraction time， 35 min. Under the optimized conditions， the proposed DES&INF-LMME-HPLC exhibited good linearity in the range of 2.86-1 000 μg/L （<i>r</i>²>0.997 2）， with limits of detection （LODs） （<i>S/N</i>=3） and limits of quantification （LOQs） （<i>S/N</i>=10） ranging from 0.86-10.0 μg/L and 2.86-33.3 μg/L， respectively. The obtained enrichment factors （EFs） ranged from 32 to 84 with recoveries of 99.4%-109.2%. The intra-day and inter-day precisions at three spiked levels （low： 30 μg/L； medium： 50 μg/L； high： 100 μg/L）， expressed as relative standard deviations （RSDs）， were no more than 4.9% and 5.3%， respectively （<i>n</i>=6）. This method has been successfully applied to the determination of four antibiotics in commercially available milk products. The spiked recoveries for the four antibiotics at high， medium and low levels ranged from 88.9% to 113.4%. The proposed method is accurate， simple， sensitive and eco-friendly， and could be a good reference to the development of new analytical method for antibiotic residues in dairy products.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"422-431"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077540/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680076","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":"[Assessment on data processing methods for nontarget identification of per- and polyfluoroalkyl substances using liquid chromatography-high-resolution mass spectrometry].","authors":"Bo-Xuan Zhang, Qin-Wen He, Bao-Cang Han, Cun-di Ma, Zhu-Jun Luo, Xiang-Zhou Meng","doi":"10.3724/SP.J.1123.2025.07011","DOIUrl":"10.3724/SP.J.1123.2025.07011","url":null,"abstract":"&lt;p&gt;&lt;p&gt;The widespread use， persistence， bioaccumulation， and toxicity of per- and polyfluoroalkyl substances （PFAS） have raised global concern. The number of PFAS types continues to grow， driven by changing industrial demands and regulatory environments. Non-target analysis using high-resolution mass spectrometry （HRMS） is an effective methodology for identifying novel and unknown PFAS in environmental matrices. The efficacy of non-target analysis is critically influenced by the data acquisition mode， peak picking algorithm， and deconvolution strategy. Using ultra-high performance liquid chromatography coupled with an Orbitrap mass spectrometer （UHPLC-Orbitrap MS）， this study aims to systematically evaluate data processing methods for non-targeted PFAS identification under data-dependent acquisition （DDA） and data-independent acquisition （DIA） modes. A clean sludge sample was spiked with 34 PFAS standards at three levels to assess method performance， alongside the analysis of three electroplating sludge samples. To compare the identification performance between DDA and DIA modes， a multi-step evaluation process was employed. Firstly， we assessed the peak picking capabilities of two widely used data processing software packages， MS-DIAL and MZmine. The key parameters for peak picking process are MS&lt;sup&gt;1&lt;/sup&gt; mass tolerance of 0.002 5 Da， MS&lt;sup&gt;2&lt;/sup&gt; mass tolerance of 0.01 Da， minimum peak height of 1 000， and retention time alignment tolerance of 0.1 min. Secondly， a comparison was made regarding DIA data deconvolution， specifically between MS2Dec algorithm and IonDecon algorithm. Finally， FluoroMatch was utilized to compare the true positive rate （TPR） and positive predictive value （PPV） of PFAS identification in both DDA and DIA datasets. In the spiked samples， the ［M-H］&lt;sup&gt;-&lt;/sup&gt; precursor ions for 33 PFAS standards and the ［M-CO&lt;sub&gt;2&lt;/sub&gt;-H］&lt;sup&gt;-&lt;/sup&gt; ion for HFPO-DA were successfully detected and manually verified across all three levels. For peak picking， MS-DIAL demonstrated superior performance， achieving a 100% detection rate in all spiked samples， outperforming MZmine. When comparing deconvolution performance for DIA data， MS2Dec algorithm and the IonDecon algorithm showed similar efficacy， although MS2Dec algorithm exhibited slightly better results for low-concentration samples. In DDA mode， the true positive rate for PFAS identification increased from 80% to 100% with rising analyte concentration， accompanied by a minimal decrease in positive predictive value. Conversely， in DIA mode， the true positive rate remained at 100% across all concentrations， but positive predictive value decreased as concentration increased， primarily due to interferences from in-source fragmentation and adduct ions. The degree of in-source fragmentation of perfluorocarboxylic acids （PFCAs） decreases with increasing carbon chain length. However， the proportion of adduct ions remains nearly constant across different PFAS， leading to false positive ide","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"432-443"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077534/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680141","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":"[Preparation of a novel polyhydroxy silica stationary phase and application in the separation of alginate oligosaccharides].","authors":"Rui-Wen Jiao, Dan-Dan Zhang, Xing-Yuan Hu, Wan-Ting Zhu, Xiang Li, Yi-di Cai, Dan-Dan Ren, Qiu-Kuan Wang, Long Wu, Hui Zhou","doi":"10.3724/SP.J.1123.2025.03006","DOIUrl":"10.3724/SP.J.1123.2025.03006","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Hyperbranched polyglycerols （HPG） represent an emerging class of dendritic polyethers characterized by a highly branched， three-dimensional architecture and a multitude of terminal hydroxyl groups. This distinctive structural configuration confers exceptional hydrophilicity， biocompatibility， and a high density of modifiable surface functionalities， thus establishing HPG as highly promising materials for the development of advanced chromatographic stationary phases. Their application is particularly relevant for the separation of polar and hydrophilic analytes， which has long posed a significant challenge in conventional reversed-phase liquid chromatography. The integration of such hyperbranched polymers with robust inorganic substrates， such as silica gel， has recently gained traction as a sophisticated materials strategy. This approach synergistically combines the superior mechanical strength and pressure resistance of the inorganic matrix with the rich surface chemistry and tunable hydrophilicity of the polymer， thereby addressing critical limitations of traditional stationary phases in hydrophilic interaction liquid chromatography （HILIC） applications.In the present study， a novel HILIC stationary phase， designated HPG-Sil 3， was synthesized through the in-situ ring-opening polymerization of glycidol monomers from the surface of aminopropyl-functionalized silica microparticles. The synthesis commenced with a meticulous silanization step to graft （3-aminopropyl）triethoxysilane （APTES） onto the silica surface， thereby introducing a uniform layer of primary amine groups. These amine functionalities served as initiation sites for the subsequent grafting-from polymerization， ensuring the formation of a covalently anchored， robust HPG layer. This covalent immobilization strategy is critical for mitigating stationary phase degradation and polymer leaching under prolonged chromatographic use， thereby guaranteeing long-term operational stability. The successful fabrication of the HPG-Sil 3 material and its physicochemical properties were thoroughly characterized using a suite of analytical techniques. Elemental analysis indicated a substantial increase in carbon and hydrogen content post-modification， providing quantitative evidence of organic polymer grafting. Fourier-transform infrared （FTIR） spectroscopy further corroborated this result， revealing signature absorption bands associated with the stretching vibrations of O-H and C-O-C ether linkages， which are characteristic of the HPG polyether structure. Thermogravimetric analysis （TGA） demonstrated the material's excellent thermal resilience， with the onset of HPG decomposition occurring above 200 ℃， a temperature window far exceeding the operational range of typical HILIC analyses. Textural properties， evaluated via nitrogen physisorption， showed a predictable decrease in specific surface area and pore volume relative to the unmodified silica substrate. This reduction is attributed to the pa","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"373-382"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077537/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680148","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":"[Binary encryption comprehensive experiment based on agarose gel electrophoresis].","authors":"Jin-Wei Duan, Lei Ma, Qian Zhao, Qian-Qian Wu, Bo-Yu Xin, Jia-Hua Yang, Yao Li, Qi-Zhao Wang","doi":"10.3724/SP.J.1123.2025.10029","DOIUrl":"10.3724/SP.J.1123.2025.10029","url":null,"abstract":"<p><p>This experiment is based on a 4-bit deoxyribonucleic acid （DNA） nanoswitch， in which specific DNA single strands trigger a \"linear-to-circular\" conformational transition. By leveraging the migration differences between the two conformations in gel electrophoresis， digital binary encoding is achieved. Different combinations of conformational switches can represent distinct information. Inspired by the \"protection-deprotection\" strategy in organic chemistry， an ribonucleic acid （RNA） protection strand is introduced to prevent the formation of the circular structure， thereby establishing an information encryption system. The system utilizes ribonuclease A （RNase A） for specific enzymatic cleavage to remove the protection， restoring information readout and establishing an RNA-regulated encryption system. By integrating DNA nanotechnology， binary encoding， and chemical protection strategies， agarose gel electrophoresis is applied throughout the entire experimental process， enabling full visualization from molecular construction to information read-write. This approach not only helps students master gel electrophoresis techniques and deepen their understanding of electrophoretic separation mechanisms and structure-activity relationships at the molecular level， but also exposes them to cutting‑edge fields such as molecular information encoding and DNA nanotechnology， effectively stimulating innovative thinking and interdisciplinary problem-solving skills.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"486-495"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077535/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680121","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 a machine learning-based ionization efficiency prediction model for per- and polyfluoroalkyl substances and its application in semi-quantitative analysis].","authors":"Shen-Zheng Sun, Yao-Yao Li, Yan Gao, Kang-Cong Li, Zhi Chen, Xiu-Qin Li, Qing-He Zhang","doi":"10.3724/SP.J.1123.2025.02012","DOIUrl":"10.3724/SP.J.1123.2025.02012","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Per- and polyfluoroalkyl substances （PFASs） represent a category of emerging contaminants of global concern in fields such as environmental science and food safety， due to their persistence， bioaccumulative properties and potential toxicity. Although screening methods for PFASs using high resolution mass spectrometry （HRMS） have been developed rapidly， the diversity of PFASs and the absence of standards pose significant challenges for quantitative analysis. In this study， 50 PFASs were analyzed by HPLC-HRMS. The ionization efficiency （IE） was calculated as the slope of the calibration curve. A quantitative structure-activity relationship （QSAR） model was developed employing machine learning to predict the ionization efficiencies of PFASs using PaDEL molecular descriptors. The model enables semi-quantitative estimation of PFASs concentrations in the absence of reference standards by incorporating predicted IE values. Eighteen critical descriptors were selected from a total of 1 444 PaDEL descriptors through the application of recursive feature elimination （RFE）. These selected descriptors encompassed topological descriptors， geometrical descriptors， autocorrelation descriptors， electrostatic and polarity descriptors. These individual descriptors including VE1_Dzv， GATS6i， JGI10， GATS1p and MATS4m were of great importance. Three algorithms including elastic net linear regression， random forest （RF）， and XGBoost were evaluated for model performance. In the elastic net linear regression model， the root mean square error （RMSE） for the training dataset was 0.049 0， and the coefficient of determination （&lt;i&gt;R&lt;/i&gt;²） was 0.993 0； for the test dataset， the RMSE was 0.163 0， with an &lt;i&gt;R&lt;/i&gt;² of 0.756 1. In the RF model， the RMSE for the training dataset was 0.163 1， and the &lt;i&gt;R&lt;/i&gt;² was 0.921 9； for the test dataset， the RMSE was 0.131 6， with an &lt;i&gt;R&lt;/i&gt;² of 0.840 9. In the XGBoost model， the RMSE for the training dataset was 0.052 1， and the &lt;i&gt;R&lt;/i&gt;² was 0.992 0； for the test dataset， the RMSE was 0.118 4， with an &lt;i&gt;R&lt;/i&gt;² of 0.871 3. Nonlinear algorithms of random forest and XGBoost demonstrated superior predictive performance compared to the elastic net linear regression， with XGBoost exhibiting best performance. Random forest， a bagging-based approach， trains individual decision trees independently and aggregates predictions through averaging. In contrast， XGBoost employs gradient boosting methodology， iteratively optimizing the model by sequentially training new trees in order to address residuals from previous iterations. The independent training mechanism of random forest inherently lacks the iterative optimization framework that is characteristic of gradient boosting. Specifically， XGBoost systematically enhances predictive accuracy by generating new trees that target residual errors from preceding models， thereby progressively refining predictive performance. This fundamental difference in optimization strategy enables XGBoost to more ef","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"444-452"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077542/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680068","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 65 synthetic cannabinoids in whole blood by QuEChERS-ultra performance liquid chromatography- mass spectrometry].","authors":"Zhang Xi, Yi Ye, Song-Pan Li, Jing Kang, Wei-Qun Liu, Jing Zhang, Dao-Xia Li","doi":"10.3724/SP.J.1123.2025.04037","DOIUrl":"10.3724/SP.J.1123.2025.04037","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Synthetic cannabinoids （SCs） have become the most diverse and widely abused class of new psychoactive substances in the world. Blood and urine are classic sample matrices for in vivo toxin analysis， but some SCs have high lipophilicity， and the concentration of parent drugs in urine is extremely low， making them difficult to detect. Metabolites need to be investigated， and SCs with similar structures can produce the same metabolites. Therefore， establishing urine detection methods and interpreting results are relatively complex. In contrast， the detection of synthetic cannabinoid parent drugs in blood is more straightforward， and detecting parent drugs in blood can serve as direct evidence in legal cases. In order to detect the abuse of SCs， a QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was developed to simultaneously determine 65 SCs in blood. The sample preparation and detection conditions were optimized. Quantification was achieved using an internal standard and matrix-matched calibration curves， enabling rapid screening and quantitative analysis of the 65 SCs in blood. Following protein precipitation with acetonitrile， the blood extract was further extracted and purified using QuEChERS reagents. Chromatographic separation of all 65 SCs was performed on a Waters Acquity UPLC HSS T&lt;sub&gt;3&lt;/sub&gt; column （100 mm×2.1 mm， 1.8 μm） maintained at 40 ℃. Detection employed dynamic multiple reaction monitoring （dMRM） mode with a mobile phase consisting of 0.1% （volume fraciotn） formic acid aqueous solution and acetonitrile， delivered at a flow rate of 0.25 mL/min. The injection volume was 2 μL. The 65 SCs exhibited good linear relationships in the mass concentration range of 0.05-200 ng/mL with correlation coefficents （&lt;i&gt;r&lt;/i&gt;） exceeding 0.992. The limits of detection （LODs） were between 0.01 and 0.2 ng/mL， and the limits of quantitation （LOQs） were between 0.05 and 0.5 ng/mL， respectively， which meet the requirements for analyzing SCs in blood sample. The intra-day and inter-day precisions （&lt;i&gt;n&lt;/i&gt;=6） were determined to be 1.0%-9.9% by spiking blank blood samples with the 65 SCs at mass concentrations of 1， 5， and 50 ng/mL. The recoveries of the 65 SCs were between 62.2% and 116.9%， and the matrix effects were between 70.2% and 117.7%. All analytes demonstrated good stability and acceptable dilution integrity in blood samples. Using the established method， 10 blood samples from suspected drug use cases were successfully screened for SCs. The target compounds were detected in all 10 samples， specifically including ADB-BUTINACA， MDMB-4en-PINACA， MDMB-FUBICA， and 5F-MDMB-PICA with mass concentrations ranging from 1.9 to 23.1 ng/mL. The detection rates of ADB-BUTINACA and MDMB-4en-PINACA were 90% and 50%， respectively， suggesting their relatively high prevalence in China's illegal drug market. In addition， two or more SCs were detected simultaneously in six blood samples. Compared with other existing l","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"393-402"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077541/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680106","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 38 antibiotic residues in honey by magnetic dispersive solid-phase extraction-liquid chromatography-tandem mass spectrometry].","authors":"Jing Sun, Yu Zhang, Feng-Mao Liu, Wen Zhao, Yue Jin, Lin Zhang, Xiao-Feng Xue, Rui Chen, Hua-Tian Zhou","doi":"10.3724/SP.J.1123.2025.07017","DOIUrl":"10.3724/SP.J.1123.2025.07017","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Accurate antibiotic residue detection in honey is crucial for food safety and veterinary drug regulation in apiculture. Honey is a particularly challenging matrix. The high sugar content， strong viscosity， and pronounced matrix effects of the sample make it difficult to extract and detect target analytes effectively. Moreover， multiple antibiotics are used in beekeeping， while existing residue standards often provide incomplete coverage. These limitations highlight the urgent need for a robust and environmentally friendly multi-residue analytical method. In this study， a green and sensitive method was developed for the simultaneous determination of 38 antibiotic residues， including chloramphenicol， quinolones， and sulfonamides， in honey. Sample preparation was based on magnetic dispersive solid-phase extraction （MDSPE） using a mixed-mode hydrophilic-lipophilic balance （mHLB） magnetic sorbent. This sorbent combines hydrophilic and hydrophobic interactions， enabling efficient extraction of chemically diverse antibiotics. Method optimization was performed systematically. A Plackett-Burman design was used to screen seven factors influencing extraction. The sorbent dosage， sample volume， and extraction time were identified as the most significant. These variables were further optimized by response surface methodology， which minimized the number of experimental runs while clarifying interactions among factors. The final protocol required only 10 mg of sorbent， 5 mL of sample extract， and 1 mL of methanol for elution. This miniaturized approach represents an environmentally sustainable method. Chromatographic separation was achieved on a Poroshell 120 SB-C18 column （100 mm×2.1 mm，2.7 μm） using a gradient of acidified methanol and water. Detection was carried out by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） with electrospray ionization operated in both positive and negative modes， and multiple reaction monitoring ensured high sensitivity and selectivity. The method was fully validated. Excellent linearity was obtained for all analytes in the range of 0.02-200 μg/L， with correlation coefficients above 0.99. Limits of detection ranged from 0.01 to 0.12 μg/kg， while limits of quantification ranged from 0.02 to 0.39 μg/kg. Recoveries at three spiked levels ranged from 70.5% to 109.3%， with relative standard deviations （RSDs） below 10.8%. Matrix effects ranged from 0.82 to 1.19， indicating effective suppression of interference and reliable quantification in complex honey samples. The method was successfully applied to 42 commercial honey batches from different geographical regions. Several antibiotics were detected， including chloramphenicol， as well as other compounds without established maximum residue limits. These findings indicate potential misuse of antibiotics in beekeeping and reveal important gaps in current regulatory frameworks， underscoring the need for continuous monitoring and timely updates to residue st","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"467-478"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077539/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680094","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 lubabegron residues in animal-derived foods by ultra performance liquid chromatography- tandem mass spectrometry].","authors":"Cheng Yang, Wei-Xia Zhu, Ya-Feng Liu, Hong-Wei Zhang, Wei Wei, Kai Hu","doi":"10.3724/SP.J.1123.2025.02006","DOIUrl":"10.3724/SP.J.1123.2025.02006","url":null,"abstract":"<p><p>Lubaberone （LUB） is the first U S Food and Drug Administration （FDA） approved feed additives for reducing gaseous emissions from animals or their wastes， and the intake of animal-derived foods is an important source of human exposure to LUB. However， the lack of applicable analytical methods makes it difficult for regulatory authorities to monitor LUB in animal-derived foods. There is an urgent need to establish efficient and accurate methods for the analysis of LUB in animal-derived foods. In this study， a method was developed for the determination of LUB from six types of typical animal-derived foods （beef， bovine liver， bovine fat， mutton， sheep liver and sheep fat） by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The effects of extraction solvent types， extraction methods， extraction time and purification cartridges on the recovery of LUB were investigated， and the optimal conditions for sample pretreatment were confirmed. The homogenized samples were extracted using 0.5% formic acid acetonitrile via ultrasonication for 10 min， and then filtered by high-speed centrifugation， and the extracted solution was cleaned using SPE with a PRiME HLB cartridge. The LUB was separated on a Shim-pack GIST C18-AQ chromatographic column （100 mm×2.1 mm， 2.7 μm） with 0.1% formic acid aqueous solution-0.1% formic acid acetonitrile as mobile phases at a flow rate of 0.3 mL/min， and detected in positive ion switching mode （ESI⁺） with multiple reaction monitoring （MRM） scanning， and quantitatively analyzed using the external standard method. Under the optimized experimental conditions， LUB in different animal-derived food matrices showed good linearity within their respective linear concentration ranges with the correlation coefficients （<i>r</i>） greater than 0.99. The limits of detection （LODs） and the limits of quantification （LOQs） were 0.4‒1.0 μg/kg and 1.0‒2.0 μg/kg， respectively. The recoveries of LUB spiked at low， medium and high levels ranged from 81.5% to 116.5% with relative standard deviations （RSDs） of 2.0%‒8.2%. The method is simple， rapid and highly sensitive， which can enable the analysis of LUB residues in animal-derived foods， and provides analytical technology support for the daily detection of LUB residues in imported and exported animal-derived foods.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"479-485"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077532/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680151","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 eight ultraviolet absorbers in surface water and wastewater by ultra performance liquid chromatography-triple quadrupole mass spectrometry].","authors":"Hui-Jing Sun, Bei-Bei Zhang, Meng-Qiao Huang, Hui Wang, Guan-Jiu Hu, Hui-Min Chen","doi":"10.3724/SP.J.1123.2025.08001","DOIUrl":"10.3724/SP.J.1123.2025.08001","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Ultraviolet （UV） absorbers are a group of chemicals widely used in various industrial and consumer products， such as plastics， coatings， and personal care products， to protect against UV radiation. Among them， benzotriazole derivatives （e.g. UV-326， UV-327， UV-328， UV-329， and UV-P） are the most frequently employed. Owing to their widespread use and potential persistence in the environment， these compounds have been detected in various environmental matrices， including surface water， wastewater， sediment， and biota. Certain UV stabilizers have been reported to exhibit endocrine-disrupting properties and pose potential ecological risks. Therefore， developing sensitive and reliable analytical methods for monitoring these compounds in environmental samples is essential. To address the need for reliable detection methods， this study developed a robust method based on liquid-liquid extraction （LLE） coupled with ultra performance liquid chromatography-triple quadrupole mass spectrometry （UPLC-MS/MS） for the simultaneous determination of eight UV absorbers in surface water and wastewater. Critical optimization of the pretreatment process focused on solvent selection and purification parameters. The finalized protocol involved extracting 100 mL water samples twice with dichloromethane. After nitrogen-assisted solvent evaporation， the residue was reconstituted in methanol and mixed with the internal standard solution. UPLC-MS/MS parameters were optimized to achieve optimal instrumental performance. The separation of the eight UVs was performed using a BEH C18 column （100 mm × 2.1 mm， 1.7 μm） with a gradient elution system consisting of 0.2% （mass fraction） formic acid aqueous solution and acetonitrile at a flow rate of 0.4 mL/min. The injection volume was 2 μL. Detection was performed in positive ion mode using multiple reaction monitoring （MRM）， with an electrospray ionization voltage set at 5 500 V. Quantification was achieved via internal standard calibration to ensure precision and accuracy. The method demonstrated excellent linearity for all target compounds across their respective concentration ranges， with a correlation coefficient （&lt;i&gt;r&lt;/i&gt;）&gt;0.995. The method detection limits （MDLs） ranged from 1.3 ng/L to 2.8 ng/L， indicating high sensitivity. Recovery tests conducted at low， medium， and high spiking levels （20， 200， and 800 ng/L） yielded recoveries of 80.3%-117.8%， with relative standard deviations （RSDs） of 1.4%-10.5%， confirming the method's robustness across different sample matrices. Application of the method to 10 textile dyeing wastewater samples revealed the presence of four UV absorbers： UV-329， UV-326， UV-328， and UV-350. Notably， UV-329 showed the highest detection frequency and accounted for 85% of the total detected mass concentrations， ranging from 5.2 to 2 109 ng/L. Its prevalence suggests its widespread use in industrial processes and potential persistence in aquatic environments. In conclusion， the developed method is highl","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"413-421"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077533/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680086","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}