Se pu = Chinese journal of chromatography最新文献

{"title":"[Determination of two pancreatic stimulants in equine urine using ionic liquid-based deep eutectic solvent-assisted liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry].","authors":"Qian Chen, Zhi-Chao Ma, Yao-Nan Li","doi":"10.3724/SP.J.1123.2025.03019","DOIUrl":"10.3724/SP.J.1123.2025.03019","url":null,"abstract":"<p><p>Acetohexamide （AH） and chlorpropamide （CP） can stimulate pancreatic secretion of insulin and regulate water-salt balance， which may indirectly lead to an increase in adrenaline and potentially enhance the athletic performance of horses. For the protection of horse welfare and the consideration of fair competition， AH and CP were listed as pancreatic stimulants by the Federation Equestre Internationale （FEI）. A method for the detection of pancreatic stimulants in equestrian sports needs to be established. Before analyzing these drugs from biological samples such as urine， it is necessary to perform pre-treatment to separate and concentrate the target analytes. However， there are several disadvantages to using traditional pre-treatment methods， including toxicity and inefficiency. A rapid and environmentally friendly pre-treatment method utilizing ionic liquid-based deep eutectic solvent vortex-assisted liquid-liquid microextraction （IL-DES-VALLME） was developed. Coupled with ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS）， the approach enabled efficient extraction and sensitive quantification of AH and CP from equine urine. <i>N-</i>Butyl-<i>N-</i>methylmorpholinium bis（（trifluoromethyl）sulfonyl）imide （EMMPNTF<sub>2</sub>） was chosen as the hydrogen bond acceptor （HBA）， combined with pentafluorophenol （PFP） acting as the hydrogen bond donor （HBD）. A molar ratio of 1∶4 （HBA/HBD） was identified as the optimum composition of IL-DES. Differential scanning calorimetry （DSC） was utilized to measure the melting point of the synthesized IL-DES. Fourier-transform infrared （FT-IR） spectra and proton nuclear magnetic resonance （<sup>1</sup>H NMR） spectra were employed to characterize the structure of the IL-DES and investigate the hydrogen bonding interactions between its components. Under the optimum conditions， only 100 μL of IL-DES， 1 mL of equine urine， and 6 min were required. An external standard calibration method was utilized for quantification， and a linear relationship was achieved with a mass concentration range of 0.2-20 000 ng/mL for AH and 0.5-20 000 ng/mL for CP. The coefficients of determination （<i>r</i><sup>2</sup>） were all greater than 0.999. The limits of detection （LOD） of the method based on a signal-to-noise ratio of 3 were 0.1 ng/mL for AH and 0.2 ng/mL for CP. The limits of quantification （LOQ） of the method based on a signal-to-noise ratio of 10 were 0.2 ng/mL for AH and 0.5 ng/mL for CP. The absolute values of matrix effects were all less than 20% （-8.9% for AH， -11.2% for CP）. Method accuracy， assessed through recovery studies at multiple concentrations across the linear range， yielded values between 90.2% and 110.4%. Precision， expressed as relative standard deviation （RSD）， was excellent， with intra-day RSDs≤6.6% and inter-day RSDs≤5.8%. The RSDs for robustness were less than 5.7%， and the average carry-over ratios were in the range of 11.4%-17.3%， indicating good method robustness and ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 9","pages":"1038-1047"},"PeriodicalIF":0.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13586920/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148993497","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 15 fentanyl analogs and amphetamine-type stimulants in hair by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry].","authors":"Qi Wei, Fu-Hai Su, Xin Zhu","doi":"10.3724/SP.J.1123.2025.12005","DOIUrl":"10.3724/SP.J.1123.2025.12005","url":null,"abstract":"<p><p>Drug abuse is a major global public health problem. Fentanyl analogs and amphetamine-type stimulants （ATS） are widely abused worldwide. Hair analysis can trace drug use history over months. This technique has unique advantages in forensic toxicology. However， its application is limited by a lack of matrix-certified reference materials （CRMs）. At present， the existing CRMs are unable to simultaneously cover both fentanyl analogs and amphetamine-type stimulants. This study established a hair sample preparation method based on a water‑dimethyl sulfoxide‑hydrochloric acid soaking approach， targeting 15 analytes （nine fentanyl analogs and six ATS）. The soaking time was systematically investigated. Drug incorporation into hair reached a maximum at 24 days. A slight decrease was observed at 25 days. This decrease may result from desorption and solvent-induced structural changes in keratin. Therefore， 24 days was selected as the optimal soaking time. Preparation experiments demonstrated that 14 of the 15 drugs were successfully embedded into the hair matrix. This study also applied a dual-platform quantitative strategy for certification. The two platforms were liquid chromatography-tandem mass spectrometry （LC-MS/MS） and gas chromatography-mass spectrometry （GC-MS）. Cross-validation between the two platforms improved the reliability of certified values. Sample pretreatment conditions were optimized using Box-Behnken response surface methodology. Four factors were investigated： extraction temperature， extraction time， liquid-to-solid ratio， and hydrochloric acid concentration. The effects of the four factors on extraction efficiency followed a decreasing order： extraction temperature>extraction time>liquid-to-solid ratio>hydrochloric acid concentration. The optimal extraction conditions were as follows： extraction temperature 40 ℃， extraction time 50 min， liquid-solid ratio 100∶1 （mL/g）， and hydrochloric acid concentration 0.01 mol/L. Method validation was performed according to international guidelines. For LC-MS/MS， the limits of detection （LODs） and quantification （LOQs） were 0.05 pg/mg and 0.25 pg/mg， respectively. For GC-MS， the LODs and LOQs were 0.02 ng/mg and 0.08 ng/mg， respectively. Good linearities were obtained for all 15 drugs. Correlation coefficients （<i>r</i>） were greater than 0.999 for both platforms. Good linearities were obtained for all 15 analytes on both platforms with correlation coefficients >0.999 over the respective concentration ranges Intra-day precisions （<i>n</i>=6） were evaluated as relative standard deviations （RSDs）. Inter-day precision （<i>n</i>=30 over 5 days） was also calculated. For 14 drugs （except amphetamine）， RSD values ranged from 0.2% to 9.4%. All RSDs were below 10%， indicating good repeatability and intermediate precision. Stability of hair extracts was assessed at 1， 24， 48， 72， and 96 h at room temperature. The extracts were stable for at least 96 h when stored at room temperature， with RSDs below 6.0%","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 9","pages":"1048-1058"},"PeriodicalIF":0.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13586919/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148993544","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 and performance testing of a high-sensitivity pulsed flame photometric detector].","authors":"Jun-Bin Chen, Hao-Yuan Cai, Zhi-Han Deng, Yu-Jie Jin, Jian-Hai Sun","doi":"10.3724/SP.J.1123.2026.03027","DOIUrl":"10.3724/SP.J.1123.2026.03027","url":null,"abstract":"<p><p>The conventional flame photometric detector （FPD） is widely used for sulfur-selective gas chromatography. However， the FPD is sensitive to hydrocarbon backgrounds. Its sulfur response also depends strongly on flame stability. These factors limit stable trace sulfur determination in complex matrices. A pulsed flame photometric detector （PFPD） provides a time-resolved approach to this problem. Sulfur emission appears later than most hydrocarbon background emissions after pulsed combustion. A suitable acquisition window can therefore improve sulfur selectivity. In this study， a high-sensitivity single-channel PFPD was designed and tested. The aim was to establish reproducible operating conditions for trace sulfur analysis. The detector consisted of five functional modules： the combustion and ignition module， the gas supply module， the optical collection and detection module， the temperature-control module， and the mechanical support and sealing module. The combustion zone consisted of a vertically mounted quartz chamber. The chamber had an outer diameter of 4 mm. Its inner diameter was 2 mm. Its total length was 17.5 mm. The effective combustion length was 12 mm. The calculated chamber volume was 37.68 mm<sup>3</sup>. Numerical simulation was used to examine flame propagation and self-extinction. A 12 mm effective length maintained a stable finger-shaped flame front. The flame was self-terminated near the lower limiting orifice at about 1.97 ms. The hydroxyl radical mass fraction decreased close to baseline within 5 ms， whereas the temperature decayed more gradually and approached its initial level at approximately 30 ms. These results supported the chamber design for periodic pulsed combustion. The optical unit used a quartz light guide and a BG-12 band-pass filter. The filter matched the sulfur emission band near 394 nm. A photomultiplier tube （PMT） recorded the time-resolved emission signal. Two electronic pneumatic control （EPC） units were used for gas regulation. One unit controlled hydrogen and air for the ignition chamber. The other unit controlled hydrogen and air for the combustion chamber. This design separated ignition conditions from analytical combustion conditions. It also reduced uncertainty caused by coupled gas adjustment. The optimization started with the ignition chamber. Then the combustion chamber was optimized under the fixed ignition baseline. Finally， detector temperature and PMT voltage were evaluated. Peak area， sensitivity， and signal-to-noise ratio （SNR） were used as indicators. Gas chromatographic tests used a sulfur-specific quartz capillary column. Nitrogen was used as the carrier gas. The gate delay was 6 ms. The gate width was 18 ms. The trigger level was 500 mV. A stable pulsed flame was obtained at an ignition-chamber hydrogen flow of 8.0 mL/min. The corresponding ignition-chamber air flow was 19.0 mL/min. Under this ignition baseline， the combustion chamber was further adjusted. A higher sulfur response was ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 9","pages":"1059-1073"},"PeriodicalIF":0.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13586926/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148993567","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 33 non-steroidal anti-inflammatory drug residues in horse urine by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Xiao-Nan Zhang, Zhi-Chao Ma, An Liu, Yuan Huang, Xue-Hong Min, Mei Liu, Zheng-Qi Xie, Yan-Song Wei","doi":"10.3724/SP.J.1123.2025.08014","DOIUrl":"10.3724/SP.J.1123.2025.08014","url":null,"abstract":"<p><p>Non-steroidal anti-inflammatory drugs （NSAIDs） are often used to treat horses' injuries and pain due to long-term training and competitions. In equestrian competitions， NSAIDs do not affect the upper limit of a horse's athletic ability， but they can enable the horse to perform close to its maximum capacity by reducing inflammation and pain. This not only affects the competition results， but also fails to ensure the health and welfare of the horses. Therefore， it has become crucial to effectively monitor and control NSAIDs residues during equestrian competition. In this study， a rapid screening and determination method for 33 NSAIDs in horse urine was established using QuEChERS pretreatment combined with ultra performance liquid chromatography-tandem mass spectrometry （QuEChERS-UPLC-MS/MS）. The pretreatment process， chromatographic conditions， and mass spectrometric conditions were also optimized. In brief， the target analytes in 1 mL of horse urine samples were extracted with 5 mL of acetonitrile. During extraction， 100 mg of NaCl was added as a salting-out agent， and the mixture was shaken for 3 min. Subsequently， the extract was purified using a QuEChERS method with 300 mg of anhydrous MgSO<sub>4</sub>， 40 mg of octadecylsilane-bonded silica （C<sub>18</sub>）， and 40 mg of primary secondary amine （PSA） as sorbents. After centrifugation， the supernatant was dried under nitrogen and reconstituted. The 33 NSAIDs were separated on an Agilent Poroshell 120 EC-C<sub>18</sub> analytical chromatographic column （100 mm×3.0 mm，2.7 μm） with gradient elution using （A） 0.1% formic acid aqueous solution and （B） methanol solution as the mobile phases. The gradient elution program was as follows： 0-1 min， 30%B； 1-3 min， 30%B-60%B； 3-12 min， 60%B-85%B； 12-12.1 min， 85%B-95%B； 12.1-14 min， 95%B； 14-14.1 min， 95%B-30%B； 14.1-17 min， 30%B. Then， the target analytes were determined by UPLC-MS/MS in dynamic multiple reaction monitoring （dMRM） mode with positive/negative ion switching. Quantification was performed using the matrix-matched external standard method. The results showed that the method can rapidly and simultaneously determine the 33 NSAIDs in horse urine. The analytes had good linear relationships within their respective ranges， with correlation coefficients of >0.99. The limits of detection （LODs） and quantification （LOQs） were 0.1-1.0 μg/L and 0.9-5.4 μg/L， respectively. The recoveries of the 33 NSAIDs in horse urine were between 70.8% and 123.8% at three spiked levels of LOQ， 20 μg/L and 200 μg/L. The relative standard deviations of all targeted compounds ranged from 1.9% to 14.8%. The method was applied to 10 actual horse urine samples. The results revealed the presence of three NSAIDs， including ketorolac， lornoxicam and naproxen， with contents ranging from < LOQ to 6.87 μg/L. According to the Equine Prohibited Substances List published by the Federation Equestre Internationale （FEI）， ketorolac and naproxen are controlled medications. They are ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 9","pages":"1028-1037"},"PeriodicalIF":0.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13586922/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148993491","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":"[Open experiment of modern instrumental analysis course： preparation of biomass-derived functional materials and their enrichment application of antibiotics in water environment].","authors":"Xiao-Yun Lei, Ling-Xia Jin, Xiao-Ping Wu","doi":"10.3724/SP.J.1123.2025.10028","DOIUrl":"10.3724/SP.J.1123.2025.10028","url":null,"abstract":"<p><p>To cultivate systematic thinking and innovation capabilities in senior undergraduate students majoring in chemistry and related fields， this project proposes an open-ended experiment that focuses on the preparation， characterization， and application of biomass-derived functional materials. The experiment incorporates essential procedures such as the preparation of biochar materials and the polymer synthesis. Characterization of the material's structure and hydrophilicity/hydrophobicity is performed using scanning electron microscopy， infrared spectroscopy， and water contact angle measurements. During the application phase， the self-prepared materials are utilized to adsorb glycopeptide antibiotics from real water samples， followed by quantitative analysis using high performance liquid chromatography. Throughout the experiment， students will enhance their ability to integrate multidisciplinary knowledge， master skills across the entire analytical workflow-from sample pretreatment to instrumental analysis-while also improving their competencies in material preparation， instrument operation， and data analysis. Through this hands-on practice， students will develop a practical understanding of the application of analytical technologies in environmental remediation and monitoring， thereby strengthening their innovative capacity to identify and solve complex chemical problems. Furthermore， the implementation of this open-ended experiment contributes to advancing the resource utilization of biomass materials， aligning with the demands of a low-carbon economy.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 9","pages":"1082-1089"},"PeriodicalIF":0.0,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13586916/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148993576","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 chemical constituents and bioavailable components in Yupingfeng Granules using ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry].","authors":"Wen-Sen Lu, Guan-Lin Xiao, Min-Shan Wu, Jia-Ying Wu, Quan Liu, Ai-Li Xu","doi":"10.3724/SP.J.1123.2025.11008","DOIUrl":"10.3724/SP.J.1123.2025.11008","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Yupingfeng Granules， a classical and widely prescribed formula in traditional Chinese medicine， is extensively employed in clinical practice for its well-documented immunomodulatory and preventive activities. However， the highly complex chemical composition of this multi-herb formula and the specific material basis responsible for its therapeutic effects in vivo remain inadequately characterized and systematically elucidated. Research on its pharmacokinetically critical blood-entering components， which are indicative of systemic exposure and potential direct activity， particularly under representative pathological conditions， remains notably scarce and insufficient. This study therefore aims to systematically characterize the comprehensive chemical profile of Yupingfeng Granules by employing advanced analytical techniques such as HPLC-MS. Furthermore， it seeks to comprehensively investigate and characterize its blood-entering components specifically in cyclophosphamide-induced immunodeficient rat models， comparing them with normal physiological conditions where applicable. The overarching objective is to identify， quantify， and shed light on the formula's potential active constituents that reach the systemic circulation. This work is expected to provide a more solid and detailed scientific basis for a deeper， molecular-level understanding of the pharmacodynamic mechanism of this important traditional Chinese medicine preparation and to inform its future rational clinical application and quality control. An ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF MS） technology was used to identify the chemical composition of Yupingfeng Granules and the plasma-entering components after administration to immunodeficient model rats. The prepared granule and serum samples were analyzed using a Waters CORTECS UPLC C18 column （150 mm×2.1 mm， 1.6 μm） with gradient elution of 0.1% formic acid aqueous solution and acetonitrile as the mobile phases. The flow rate was set at 0.3 mL/min， the column temperature was maintained at 35 ℃， and the injection volume was 3 µL. Data were acquired in both positive and negative ion modes using an electrospray ionization source. The identification of chemical constituents was performed by comparing retention times， accurate relative molecular masses， and MS/MS fragment ions with those of reference standards， along with reference to relevant literature. Through a systematic analysis involving comparison of retention times， accurate molecular weights， and MS/MS fragment ions， combined with cross-referencing against relevant literature and authenticated reference standards， the chemical profile of Yupingfeng Granules and the bioactive components absorbed in vivo were comprehensively characterized. The investigation successfully identified a total of 52 chemical constituents in Yupingfeng Granules. Furthermore， 11 bioavailable components were detected in rat plasma after administr","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"911-923"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425208/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149170315","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 methods and technological advancements in herbal material science].","authors":"Yan-Fang Liu, Han Zhou, Ji-Xia Wang, Ai-Jin Shen, Dian Liu, Yang Han, Wen-Yi Yu, Bin Yuan, Zhen Wang, Jie Zeng, Xing-Ya Xue, Jia-Tao Feng, Zhi-Mou Guo, Xin-Miao Liang","doi":"10.3724/SP.J.1123.2026.03008","DOIUrl":"10.3724/SP.J.1123.2026.03008","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Traditional Chinese medicine （TCM）， as a complex system of substances， has long faced the challenges of an unclear material basis and obscure mechanisms of action， which has hindered its modernization and internationalization. To address these challenges， the \"Herbalome\" project was launched in 2007. This initiative aims to systematically reveal the material composition， structure， and biological functions of TCM through the integration of multidisciplinary technologies， thereby elucidating the synergistic mechanisms of multi-component and multi-target interactions. This paper reviews key methodological and technological advancements in the field of herbal material science. Specifically， regarding the composition and structural identification of herbal compounds， the integration of liquid chromatography-mass spectrometry with two-dimensional chromatography and intelligent data mining strategies has enabled high-throughput characterization of the complex chemical constituents of TCMs， as well as the discovery of novel compounds. Furthermore， advancements in multidimensional high-performance preparative chromatography and the development of novel multidimensional multi-channel separation and purification devices have overcome bottlenecks in the large-scale systematic preparation of TCM compounds. Additionally， nuclear magnetic resonance technology， enhanced by artificial intelligence techniques， such as intelligent heteronuclear single quantum coherence （HSQC） recognition and deep learning models， has significantly improved the efficiency and accuracy of structural identification. In the study of the biological effects of herbal substances， target-oriented and phenotype-oriented pharmacological technologies， such as cellular label-free integrative pharmacology， thermal proteome profiling， and affinity mass spectrometry， have facilitated the discovery of targets and the elucidation of mechanisms for bioactive components in TCM. Moreover， TCM databases and computational simulation techniques， including virtual screening， molecular dynamics， and artificial intelligence prediction models， have supported the construction and simulation of complex \"multi-component and multi-target\" interaction networks. Structural biology techniques， particularly cryo-electron microscopy， have provided atomic-level insights into the interactions between TCM bioactive components and target proteins， advancing our understanding of structure-activity relationships and multi-target mechanisms. In conclusion， the synergistic advancement of various techniques， including separation analysis， bioeffect evaluation， and computational modelling， is driving a paradigm shift in herbal material science from \"experience-dependent\" to \"data-driven\" approaches. The ongoing emergence and integration of novel technologies will continue to reveal unexplored areas within traditional Chinese medicine， systematically elucidate its multi-component， multi-target synergistic mechanisms， and","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"847-863"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425200/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149168297","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 solvents modified reversed-phase liquid chromatography for the separation of natural products].","authors":"Hui Zhang, Hui-Min Wu, Qun He, Tianxue Qin, Su-Ying Guo, Wen-Jing Li, Rong Jiang, Guang-Ying Sun","doi":"10.3724/SP.J.1123.2026.04013","DOIUrl":"10.3724/SP.J.1123.2026.04013","url":null,"abstract":"&lt;p&gt;&lt;p&gt;The composition of natural products is usually very complex. During the separation of natural products， high loading capacity and satisfactory chromatographic resolution are often hardly achieved. To address this limitation， various modifiers were added in the mobile phase to alter the chromatographic behavior. Here， deep eutectic solvents （DESs） were chosen to accomplish this objective on C18 column. Changes in retention factor， overloaded peak shape and adsorption capacity were systematically investigated and interpreted. The application potential of DESs in the separation of natural products was then evaluated. For ionizable compounds， the addition of DESs could compress the peak width and enhance the resolution. This is closely related to the electrostatic interactions provided by hydrogen bond acceptor （HBA） of DESs. For ionizable basic compounds like nortriptyline hydrochloride， they could remain in a cationic state constantly. Consequently， ion-exchange interactions occurred between nortriptyline cation and residual silanol anion， which resulted in severe peak tailing. However， this interaction could be shielded by the addition of HBA of DESs （such as choline chloride （ChCl））. As the pH of the mobile phase increased， the dissociation of silanol groups was enhanced. This rendered the shielding effect more prominent and led to a higher peak compression of nortriptyline hydrochloride. Notably， although the mobile phase was acidic， the dissociation of silanol groups cannot be completely suppressed. It means that this modulating effect of HBA never disappears. Based on these principles， the semi-preparative separation of berberine from &lt;i&gt;Coptis chinensis&lt;/i&gt; extracts was successfully improved. The improvement in the separation of acidic compounds by DESs depends on the ion-pair formation. This effect is highly correlated with the mobile phase pH and salt concentration. Here， benzoic acid was chosen as a model to investigate the overload behavior and adsorption. The results indicated that under neutral conditions， ChCl addition converted the sigmoidal adsorption to a linear type. It can be attributed to the ion-pair formation between benzoate anions and HBA cations. Mutual repulsion between benzoate anions was therefore reduced and adsorption capacity correspondingly enhanced. Furthermore， the results of the overload experiment indicated that ChCl can effectively weaken the solute-solute interactions. It is worth noting that the mobile phase pH is barely influenced after the addition of ChCl. Remarkably， these features are of critical importance for the optimization of preparative chromatographic methods. The beneficial effect of HBAs was validated in the semi-preparative separation of chlorogenic acid from &lt;i&gt;Lonicera japonica&lt;/i&gt; extracts. For neutral compounds like morroniside， the HBA in DESs cannot affect their chromatographic behavior through electrostatic interactions. However， there are usually many ionizable impurities surroundin","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"946-959"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425206/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149166018","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":"[Recent advances on bioaffinity fishing technology for discovery of active components from natural products].","authors":"Qing-Li Qu, Xiao-Fang Wang, Duo-Long DI, Dong Pei","doi":"10.3724/SP.J.1123.2025.08021","DOIUrl":"10.3724/SP.J.1123.2025.08021","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Natural products have consistently served as an invaluable source for novel drug development， and the efficient and targeted screening of bioactive constituents from these complex mixtures is crucial for advancing drug discovery. Bioaffinity fishing techniques exploit the highly specific interactions between ligands and their biological targets-such as antigen-antibody， enzyme-substrate， and hormone-receptor interactions-to simultaneously separate and identify active compounds from complex natural product extracts. When coupled with liquid chromatography-mass spectrometry， bioaffinity fishing enables the integrated separation， screening， and analysis of bioactive molecules in a single step. This comprehensive review focuses specifically on bioaffinity fishing materials， which are fundamental to the effectiveness and reproducibility of the fishing process. The review systematically explores recent advances over the past three years， categorizing the discussion along two primary dimensions： carrier materials and immobilization methods. In terms of carrier materials， the article provides a comprehensive review of both carrier-free and carrier-based systems. Carrier-free approaches， including affinity ultrafiltration and size exclusion chromatography， utilize free targets in solution， while carrier-based systems immobilize the target onto a solid support. The review details a wide spectrum of innovative supports such as magnetic beads， which facilitate easy separation； metal-organic frameworks， known for their high surface area and tunable porosity； silica-based materials （e.g.， mesoporous silica and silica chromatographic stationary phases）， prized for their stability and versatility； gel-based materials like agarose and synthetic polymers， which offer superior biocompatibility； microchannel-based systems， including capillary columns and microfluidic chips that enable high-throughput screening with minimal sample consumption； fluorescent materials that integrate fishing with real-time activity monitoring and imaging； and other emerging materials such as graphene， carbon nanotubes， and paper-based substrates. Each material system is evaluated regarding its preparation， advantages， limitations， and representative applications in fishing active ingredients from natural products. Regarding immobilization strategies， the review compares three principal methodologies： physical adsorption， which is simple but often prone to leakage and low efficiency； physical encapsulation， which protects the target yet may incur mass transfer limitations and potential activity loss； and chemical cross-linking， which enhances stability but risks altering the target's conformation and activity. A significant portion of the discussion is devoted to advanced directional immobilization techniques designed to preserve biological activity and improve efficiency. These include various bioorthogonal reactions such as Halo-tag/alkyl chloride， His-tag/Ni-NTA， SpyTag/SpyCatche","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"900-910"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425207/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149169273","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 the key characteristic components in ginger from different origins by internal extractive electrospray ionization mass spectrometry].","authors":"Hui-Ting Wang, Si-Yu Xie, Jing-Jing Xie, Ruo-Tian Wu, Man-Man Qin, Huan-Wen Chen","doi":"10.3724/SP.J.1123.2025.09001","DOIUrl":"10.3724/SP.J.1123.2025.09001","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Ginger， the fresh rhizome of &lt;i&gt;Zingiber officinale&lt;/i&gt; Rosc. from the Zingiberaceae family， is highly valued worldwide for its unique aromatic profile and distinct pungent flavor. It is widely utilized both as a culinary spice and a natural food additive. Globally， ginger comprises 53 known genes and approximately 1 300 varieties， predominantly cultivated in tropical and subtropical regions. Major producing countries include India， China， Indonesia， and Nigeria， with China ranking as the second-largest producer. In many Asian countries， such as China， Korea， and Japan， ginger has long been recognized not only for its culinary applications but also for its medicinal properties. It is traditionally employed to alleviate cold symptoms， promote body warmth， reduce nausea， suppress coughs by clearing phlegm， and even neutralize toxins from seafood consumption. The efficacy and safety of ginger as a medicinal herb are largely determined by the content and purity of its active constituents， such as gingerols and shogaols. Thus， accurate quality assessment is essential to ensure its therapeutic value. Moreover， the contents of these bioactive compounds can vary considerably depending on the geographical origin. In China， high-quality medicinal ginger is primarily cultivated in provinces such as Yunnan， Sichuan， Guizhou and Henan. Given the complexity and diversity of ginger's chemical composition， it is crucial to understand its characteristic components and their variation with origin. This knowledge supports not only accurate quality evaluation but also reliable traceability of ginger sources. Ultimately， it facilitates the selection of ginger with superior medicinal properties for direct use in traditional medicine or as high-quality raw material in pharmaceutical development. However， conventional analytical techniques for determining origin and quality， such as high performance liquid chromatography （HPLC） and gas chromatography-mass spectrometry （GC-MS）， are often time-consuming， require extensive sample preparation， and consume large volumes of solvents. To overcome these limitations， this study developed a high-throughput method based on internal extractive electrospray ionization mass spectrometry （iEESI-MS） for rapid compositional profiling and origin authentication of ginger. Samples were collected from four major ginger-producing regions in China： Yunnan， Sichuan， Guizhou， and Henan. Each sample was minimally processed into fragments， with only 5.0 mg used for analysis. The fragments were placed on a filter membrane inside a custom-built iEESI-MS device. Key instrumental parameters such as the extraction solvent composition， ion transfer tube temperature， spray voltage， and solvent flow rate were systematically optimized to enhance detection sensitivity and reproducibility. Under optimal conditions， real-time extraction and ionization of chemical constituents from ginger tissue were achieved， yielding representative mass spectral finge","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"968-978"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425202/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149169342","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}