Se pu = Chinese journal of chromatography最新文献

{"title":"[Research advances in the preparation and structural characterization of depolymerized oligosaccharides from traditional Chinese medicine].","authors":"Jun-Yi Liu, Yi Zheng, Jing-Yu Yan","doi":"10.3724/SP.J.1123.2025.08024","DOIUrl":"10.3724/SP.J.1123.2025.08024","url":null,"abstract":"<p><p>Polysaccharides derived from traditional Chinese medicine （TCM） have attracted widespread attention due to their excellent bioactivities， such as immunomodulatory， anti-inflammatory， and anti-tumor effects. However， these polysaccharides exhibit inherent characteristics including large molecular weights， complex monosaccharide compositions， and diverse branched structures. These features result in low bioavailability and difficulties in unraveling their structure-activity relationships （SARs）， thereby imposing significant limitations on their practical applications. In contrast， oligosaccharides possess distinct advantages： they have low molecular weights， relatively simple structures， and are easy to purify and characterize structurally. Owing to these properties， oligosaccharides serve as ideal models for deciphering the SARs of TCM polysaccharides. Consequently， the preparation， separation and purification， and structural characterization of TCM oligosaccharides have become the core research focuses in this field.This paper firstly reviews various degradation strategies from the perspective of degradation approaches. These strategies include chemical hydrolysis， oxidative degradation， enzymatic hydrolysis， and assisted degradation methods. For each method， a comparative analysis of their degradation mechanisms， product distribution characteristics， and applicable scopes is conducted. Meanwhile， it elaborates on the modification effects of different methods on the degree of polymerization （DP）， anomeric configuration， and branched structure of oligosaccharides， as well as their potential regulatory roles in the bioactivities of oligosaccharides. Subsequently， this paper carries out a systematic review on the chromatographic techniques commonly used for the separation and purification of degraded oligosaccharides， including gel filtration chromatography （GFC）， ion-exchange chromatography （IEC）， hydrophilic interaction chromatography （HILIC）， and porous graphitized carbon chromatography （PGC）. For each chromatographic technique， this paper provides a detailed account of its separation principle， applicable scenarios， and specific applications in the separation of degraded oligosaccharides. Finally， regarding the oligosaccharide structural characterization techniques-such as monosaccharide composition analysis， methylation analysis， and nuclear magnetic resonance （NMR） spectroscopy-the paper clarifies the complementarity between different techniques and their respective limitations.In summary， this paper focuses on the application of combined strategies-such as chemical hydrolysis， enzymatic hydrolysis， and physicochemical hybrid methods-in the preparation of degraded oligosaccharides derived from TCM， as well as the roles and key points of separation techniques and characterization techniques in structural elucidation. Looking ahead， the preparation， separation and purification， and structural analysis of TCM oligosaccharides require the fu","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"889-899"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425199/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149169561","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 high-performance chromatographic materials and their application in herbalome research since 2020].","authors":"Jing Feng, Dong-Hai Xia, Chun-Ying Song, Yi Qi, Gao-Wa Jin, Yan-Fang Liu, Xin-Miao Liang, Dong-Ping Yu, Zhi-Mou Guo","doi":"10.3724/SP.J.1123.2025.08025","DOIUrl":"10.3724/SP.J.1123.2025.08025","url":null,"abstract":"<p><p>Traditional Chinese medicine （TCM）， a treasured cultural heritage of the Chinese nation， plays a significant role in treating various diseases. However， the extreme complexity of its chemical components makes the comprehensive elucidation of the material basis and pharmacological mechanisms a major challenge in modern TCM research. To deeply investigate the material basis of TCM and interpret its holistic regulation mechanism involving multiple components and targets， Liang Xinmiao and his colleagues proposed the concept of herbal materiomics， which focuses on two main research directions： the material basis （including qualitative/quantitative analysis and isolation of active compounds） and the functional mechanisms （in-depth study of biological effects and modes of action）. In herbalome research， chromatographic analysis and preparative purification are powerful tools for deciphering the composition of complex TCM systems， with the development of novel chromatographic separation materials being a key driver of progress. This review systematically summarizes recent advances in the development of novel high performance chromatographic separation materials since 2020 and their applications in herbalome research. It focuses on three chromatographic modes： reversed-phase liquid chromatography （RPLC）， hydrophilic interaction liquid chromatography （HILIC）， and supercritical fluid chromatography （SFC）. The structural and performance characteristics of these novel materials are highlighted， along with their applications in the analysis and preparative purification of key active components such as alkaloids， flavonoids， saponins and terpenoids. In RPLC， the separation selectivity and retention capacity of the stationary phases for compounds such as alkaloids and flavonoids have been effectively enhanced through two primary strategies： first， by incorporating polar groups such as fluorine atoms， amides， carboxyl groups into the traditional C18/C8/phenyl skeletons； second， by utilizing natural product derivatives like cardanol and rosin as functional ligands. Furthermore， this approach has led to the creation of novel materials possessing orthogonal separation characteristics. In HILIC， various functionalized stationary phases have been developed， including <i>β</i>-cyclodextrin， nitrogen-containing heterocycles， core-shell structured amides， and surface-polymerized phases. These phases significantly improve the retention and separation efficiency of strongly polar compounds （e.g.， saponins， oligosaccharides） by providing abundant hydrogen bonding， electrostatic， and <i>π-π</i> interactions. In SFC， the development of novel stationary phases extends from modified functional skeletons （e.g.， phenyl） to zwitterionic and nitrogen-containing heterocyclic hydrophilic stationary phases. Additionally， mixed-mode stationary phases have been developed to effectively ameliorate the peak tailing problems associated with basic compounds. Concurrently， the emergen","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"864-876"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425205/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149172340","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":"[Separation and purification of phospholipids from Antarctic krill oil by hydrophilic interaction liquid chromatography].","authors":"Jian Pan, Lin Hong, Yan Zhang","doi":"10.3724/SP.J.1123.2026.04010","DOIUrl":"10.3724/SP.J.1123.2026.04010","url":null,"abstract":"<p><p>Antarctic krill has the largest biomass of any wild animal species on Earth. Krill oil extracted from Antarctic krill is rich in phospholipids， and is a major natural source of marine phospholipids. In marine phospholipids， eicosapentaenoic acid （EPA） and docosahexaenoic acid （DHA） are esterified at the <i>sn</i>-2 position of glycerol. This unique structural configuration endows them with the dual physiological functions of both phospholipids and <i>Ω</i>-3 polyunsaturated fatty acids. Compared with terrestrial phospholipids， marine phospholipids exhibit superior bioactivity in several key aspects， including neurotrophic support， anti-atherosclerotic effects， and lipid metabolism regulation， thereby conferring significant application value in pharmaceuticals， health foods， and functional foods. However， pharmaceutical excipient applications require phospholipid purity above 90%， a standard also required for high-end pharmaceutical formulations and active pharmaceutical ingredients. Currently， commercial krill oil products vary significantly in quality. Their total phospholipid content ranges from only 30% to 60%. Therefore， purifying phospholipids from Antarctic krill is essential. This process holds practical value for improving the quality standards of marine phospholipids. Hydrophilic interaction liquid chromatography （HILIC） separates polar compounds through multiple mechanisms， relying on polar interactions between the hydrophilic headgroups of phospholipids and the stationary phase， as well as partitioning within the water-rich layer on the stationary phase surface. In this study， a HILIC-based method was developed for the purification of phospholipids from Antarctic krill oil. Industrial-scale preparative chromatography requires stable stationary phases. Three HILIC-compatible stationary phases were systematically evaluated. These were unmodified bare silica gel， Diol （3% carbon）， and Diol-H （7% carbon）. Diol showed favorable retention and resolution. Therefore， Diol was selected as the optimal stationary phase. The superior performance of the Diol phase compared to Diol-H suggests that a moderate carbon content is crucial. Excessive hydrophobicity in Diol-H likely interfered with the specific hydrogen bonding interactions required for separating polar lipid headgroups. Ethanol and water were chosen as the mobile phases， because these solvents have low toxicity. Ethanol-water proportions were investigated to develop a three-step elution program： washing with 100% ethanol， elution with 95% ethanol， and column re-equilibration with 80% ethanol. Based on chromatographic plate and rate theories， a Diol column （250 mm×4.6 mm） was used. Isocratic elution with 95% ethanol was applied. The relationship between flow rate， theoretical plate number， and peak width was evaluated. An optimal flow rate was selected. Peak broadening under high sample loading was examined. This determined the maximum loading capacity. It was optimized at 8% of the ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"979-985"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425197/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149170686","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 of affinity ultrafiltration-liquid chromatography-mass spectrometry in screening natural active substances].","authors":"Yong-Bing Xu, Yu-Jia Niu, Ming-Quan Guo","doi":"10.3724/SP.J.1123.2025.08020","DOIUrl":"10.3724/SP.J.1123.2025.08020","url":null,"abstract":"<p><p>Medicinal plants serve as a valuable source of naturally occurring bioactive compounds， which have played a vital role in promoting human health， preventing and treating various diseases for thousands of years. However， the phytochemical profiles of medicinal plants， including traditional Chinese herbal medicines （TCHMs）， are notably complex and highly diverse， posing a tough challenge for the rapid screening and identification of their potential bioactive constituents. This challenge is central to pharmacological research and drug development efforts in medicinal plants including TCHMs. Therefore， the rapid and efficient screening of bioactive components from complex natural products has become a key research direction in academia. To address this issue， affinity ultrafiltration coupled with liquid chromatography-mass spectrometry （AUF-LC-MS） has emerged as an efficient technique that integrates affinity-based capture， ultrafiltration， and liquid chromatographic-mass spectrometric analysis to enable rapid screening and characterization of potential small-molecule bioactive compounds. Known for its low sample consumption， high specificity， exceptional sensitivity， operational simplicity and high efficiency， this approach leverages specific interactions between target molecules and chemical extracts to identify bioactive ligands from complex mixtures， making it particularly suitable for studying intricate matrices such as medicinal plant extracts and TCHM formulations. This study summarizes the principles， characteristics， and recent applications of AUF-LC-MS technology in the screening of potential active components in medicinal plants including TCHMs over the past decade （2015-2025）. Based on different levels of AUF-LC-MS screening， including compound level， single TCHM level， and TCHM formula level， a comprehensive summary is provided. AUF-LC-MS screening of single TCHM level is further analyzed and summarized based on the number of targets， including single target screening， dual-targets screening， and multi-targets screening. At the same time， comparisons were made between other different natural active substance screening approaches and the AUF-LC-MS method. In addition， it outlines prospective research directions for the further development of AUF-LC-MS with the aim of providing new insights for the study of the pharmacological substances of TCHMs and the development of new drugs.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"877-888"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425201/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149172021","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":"[Non-targeted metabolomics analysis of exosomes derived from <i>Glycyrrhiza uralensis</i>].","authors":"Yun-Jun Yao, Xu Qian, Fu-Xing Shu, Xi-Chao Song, Yuan-Yuan Dong, Lei-Lei Jin, Feng-Jian Liu, Zuen Ji, Jia Liu, Ji-Shuang Chen","doi":"10.3724/SP.J.1123.2025.12030","DOIUrl":"10.3724/SP.J.1123.2025.12030","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Exosomes are nanometer-sized secretory vesicles that play a pivotal role in mediating intercellular communication. Recently， exosomes derived from herbal medicine have garnered significant attention owing to their unique composition features and therapeutic potential. &lt;i&gt;Glycyrrhiza uralensis&lt;/i&gt;， a traditional Chinese medicinal and edible plant， is rich in flavonoids， terpenoids， polyketides， and phenolic acids. However， the long-term consequences of overharvesting and artificial cultivation have led to inconsistent quality of licorice materials. Plant tissue culture technology offers a sustainable approach to preserve medicinal plant resources， enabling year-round production independent of seasonal and environmental constraints. To address these challenges and explore the therapeutic potential of herb-derived exosomes， this study employed a laboratory-constructed temporary immersion bioreactor system （TIBS） for &lt;i&gt;G. uralensis&lt;/i&gt; cultivation and exosomes isolation. The key experimental procedures are summarized as follows： sterile buds derived from &lt;i&gt;G. uralensis&lt;/i&gt; seeds were used as explants. The callus proliferation medium consisted of Murashige and Skoog medium （MSM） supplemented with 1.18 mg/L 6-benzylaminopurine （6-BA）， 1.44 mg/L naphthaleneacetic acid （NAA） and 1.44 mg/L 2，4-dichlorophenoxyacetic acid （2，4-D）， yielding a maximum proliferation coefficient of 10.81 after 21 days. For shoot proliferation， sterile plantlets were generated on MSM medium supplemented with 1 mg/L 6-BA， 0.05 mg/L NAA， and 150 mL/L coconut milk （CM）， which produced sterile plantlets within 28 days of culture. When cultured in the TIBS system with an immersion frequency of 5 min every 6 h， the callus proliferation coefficient reached 13.12 after 28 days of culture. Exosomes were successfully isolated from the TIBS-cultured &lt;i&gt;G. uralensis&lt;/i&gt; calli using differential centrifugation and ultracentrifugation protocols. Comprehensive characterization was performed to validate the identity， purity， and stability of isolated exosomes. Morphological observation via transmission electron microscopy （TEM） revealed typical cup-shaped vesicles with a distinct lipid bilayer structure， which is consistent with the canonical exosomes morphology. Dynamic light scattering （DLS） analysis determined an average hydrodynamic diameter of 56 nm. The exosomes preparation exhibited a particle concentration of 1.07×10&lt;sup&gt;12&lt;/sup&gt; particles/mL， and a zeta potential of （-15.030±3.815） mV， indicating excellent colloidal stability suitable for biological applications. To decipher the molecular cargo of these exosomes， untargeted metabolomic profiling was conducted. A total of 1 760 metabolites were identified across callus and exosomes samples， of which 1 068 differential metabolites （DMs） distinguished exosomes from parental calli. Notably， 195 DMs were significantly enriched in exosomes. KEGG （Kyoto Encyclopedia of Genes and Genomes） pathway enrichment analysis revealed enrichment","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"935-945"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425203/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149167795","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":"[Iron porphyrin metal-organic framework material for efficient enrichment of earthworm polypeptides].","authors":"Kun-Song Zhan, Ming-Zhu Tang, Ying Lin, Lin-Jun Ni, Li-Shuang Yu","doi":"10.3724/SP.J.1123.2025.11018","DOIUrl":"10.3724/SP.J.1123.2025.11018","url":null,"abstract":"<p><p>Earthworms are a commonly used animal-derived traditional Chinese medicine in China， with proteins and polypeptides as their main active ingredients. However， the existing methods for separating and detecting earthworm polypeptides have problems such as insufficient preparation capacity and poor separation reproducibility. To address these challenges， this study used the iron porphyrin metal-organic framework material PCN-222（Fe） to specifically adsorb the earthworm polypeptide component L-PeakⅡ， with an adsorption capacity of 139 mg/g. First of all， PCN-222（Fe） material was successfully prepared via the one-pot method. The earthworm protease hydrolysate was obtained through alkali extraction and acid precipitation， and trypsin enzymatic hydrolysis. Then， PCN-222（Fe） was further used as a solid-phase adsorbent and combined with liquid chromatography to rapidly separate and prepare the polypeptide component L-PeakⅡ from complex earthworm enzymatic hydrolysate of the Chinese medicine. Qualitative analysis was performed by HPLC， and quantitative analysis was conducted with a BCA assay kit. HPLC analysis of the earthworm protease hydrolysate revealed multiple chromatographic peaks. After enrichment with PCN‑222（Fe） and subsequent elution， the eluted sample exhibited fewer peaks， with a well‑defined peak appearing at a retention time of approximately 15 min. In order to obtain the optimal experimental conditions for the enrichment of earthworm polypeptides， influencing factors including enzyme hydrolysate mass concentration， pH value， elution solvent type， and elution time were investigated and optimized. The results showed that optimal enrichment was achieved by incubating at an enzymatic hydrolysate mass concentration of 3.0 mg/mL and pH of 9， followed by elution with 50% acetonitrile containing 0.2% trifluoroacetic acid for 2 h. Finally， the earthworm-derived polypeptide component was obtained using a high-pressure preparative chromatographic system， achieving a purity exceeding 95%. The integrated approach employed in this study， which combines PCN-222（Fe） material with preparative chromatography， enables the efficient preparation of the target polypeptide L-PeakⅡ from medicinal earthworm samples. This strategy provides a valuable reference for the separation and purification of polypeptide components from complex animal-derived traditional Chinese medicines. Moreover， it offers a more robust， scalable， and reproducible pathway for harnessing the therapeutic potential of natural product peptides， thereby bridging the gap between traditional medicine and modern pharmaceutical analysis.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"960-967"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425204/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149170682","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":"[Isolation of angular-type pyranocoumarins from <i>Peucedani Radix</i> guided by liver microsomal metabolites and structural identification of the metabolites].","authors":"Yang Yang, Ming-Hao Liu, Hui Jin, Run-Ze Sun, Xing-Cheng Gong, Wen-Jing Liu, Yue-Lin Song","doi":"10.3724/SP.J.1123.2025.12018","DOIUrl":"10.3724/SP.J.1123.2025.12018","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Identifying the structures of metabolites is of great importance towards elucidating the therapeutic material basis of traditional Chinese medicines （TCMs）. However， current studies lack sufficient reference standards， hindering the structural identification of metabolites. This study establishes a strategy guided by the retention times and mass spectrometric information of microsomal metabolites. By coupling liquid chromatography-mass spectrometry （LC-MS） to trace and isolate target compounds from the raw materials， these compounds served as reference standards to confirm the structures of microsomal metabolites， thereby elucidating the metabolic pathways. &lt;i&gt;Peucedani Radix&lt;/i&gt; （PR， Chinese name： Qianhu） consists of the dried roots of &lt;i&gt;Peucedanum praeruptorum&lt;/i&gt; Dunn and contains abundant angular-type pyranocoumarins （APs）， which serve as primary chemical constituents and effective compound clusters as well. From the structural standpoint， C-3' and C-4' sites of APs are frequently substituted by acetoxyl， angeloxyl， isovaleroxyl and some other moieties， leading to the extensive occurrences of &lt;i&gt;regio&lt;/i&gt;-isomers， which not only possess comparable structures but also similar chemical properties. Previous studies have preliminarily unveiled that APs primarily undergo hydrolysis and acyl migration &lt;i&gt;in vivo&lt;/i&gt;， and these hydrolytic metabolites can be observed in both &lt;i&gt;in vitro&lt;/i&gt; metabolism and the raw materials. In this study， a pair of &lt;i&gt;regio&lt;/i&gt;-isomers from PR， &lt;i&gt;i.e.&lt;/i&gt;， （+）-（3'&lt;i&gt;S&lt;/i&gt;，4'&lt;i&gt;S&lt;/i&gt;）-praeruptorin A （（+）-PA） and （+）-（3'&lt;i&gt;R&lt;/i&gt;，4'&lt;i&gt;R&lt;/i&gt;）-pteryxin （（+）-Pte）， was incubated separately with human liver microsomes （HLMs） in the presence of necessary cofactors to simulate the metabolic pathways occurring &lt;i&gt;in vivo&lt;/i&gt;. After carefully processing LC-MS datasets and applying the well-defined mass fragmentation rules of APs， eight metabolites were detected and putatively identified for （+）-PA， including three hydrolysis products together with five oxidation products， whereas nine metabolites were observed and putatively identified for （+）-Pte， encompassing five hydrolysis products and four oxidation products. Noteworthily， phase I metabolism of （+）-Pte in HLMs was profiled for the first time. Various column chromatographic tools， such as silica gel column chromatography， C&lt;sub&gt;18&lt;/sub&gt; reversed-phase chromatography （ODS）， Sephadex LH-20 and semi-preparative high performance liquid chromatography equipped with achiral or chiral columns， were employed to isolate compounds-of-interest from PR extracts under the guidance of LC-MS through taking both retention time and MS/MS information into account. A total of nine AP compounds were successfully purified from PR extracts， and notably， four pairs of AP enantiomers were involved. By matching &lt;sup&gt;1&lt;/sup&gt;H- and &lt;sup&gt;13&lt;/sup&gt;C-NMR spectral information with the data archived in the literature， these compounds were identified as （3'&lt;i&gt;S&lt;/i&gt;，4'&lt;i&gt;S&lt;/i&gt;）-qianhucoumarin C （1a）， ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 8","pages":"924-934"},"PeriodicalIF":0.0,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13425198/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149169550","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Simultaneous determination of glycerol， acetic acid， and sodium bisulfite in compound amino acid injection （14AA） using ion exclusion chromatography].","authors":"Yong-Sheng Gu, Li-Min Zuo, Xiao-Li Gao, Guang-Zhi Shan, Jun Zhao","doi":"10.3724/SP.J.1123.2026.01005","DOIUrl":"10.3724/SP.J.1123.2026.01005","url":null,"abstract":"&lt;p&gt;&lt;p&gt;An ion exclusion chromatography method was established for the simultaneous determination of glycerol， acetic acid and sodium bisulfite in compound amino acid injection （14AA）. No tedious sample pretreatment is required； the sample can be directly injected after filtration through a 0.22 μm membrane filter. Chromatographic separation was achieved using an Xtimate Sugar-H column （300 mm×7.8 mm， 5 μm） packed with a strong ion-exchange resin based on a rigid styrene/divinylbenzene matrix， which is specially designed for the separation of sugar alcohols and organic acids via the ion-exclusion mechanism. The mobile phase was 7.5 mmol/L sulfuric acid solution， which was selected as it can suppress the ionization of target analytes and enhance their retention on the stationary phase； the amino groups of amino acid components undergo strong ionization， leading to no retention. Isocratic elution was adopted to ensure stable separation efficiency and short analysis time， with the flow rate set at 0.5 mL/min. Based on the ultraviolet absorption characteristics of the target analytes， 200 nm was selected as the detection wavelength. The column temperature was set at 65 ℃ and the injection volume was optimized to 10 μL， which ensures the detection sensitivity while avoiding column overload. The external standard method was adopted for quantitative analysis， featuring simple operation and reliable results. The method exhibited excellent specificity： blank solvent and negative matrix solution tests verified that amino acids caused no interference with the determination of target analytes， and the target analytes achieved good resolution from adjacent peaks. For the linearity investigation， standard solutions were prepared with linear ranges set as follows： 1.197-59.87 mg/mL for glycerol， 0.036 08-1.804 mg/mL for acetic acid， and 0.000 791 6-0.633 3 mg/mL for sulfite. Within these mass concentration ranges， the linear correlation coefficients （&lt;i&gt;r&lt;/i&gt;） of all components were greater than 0.999 5， indicating an excellent linear relationship of the method. The accuracy was verified by spiked recovery tests at three levels （80%， 100% and 120% of the labeled amount）， with three parallel preparations for each level. The results showed that the average recoveries of the target analytes ranged from 99.21% to 102.6%， with relative standard deviations （RSDs） of 0.09% to 0.86% （&lt;i&gt;n&lt;/i&gt;=3）， demonstrating the high accuracy of this method. The ion exclusion chromatography method established in this study can effectively eliminate the interference of the amino acid matrix in compound amino acid injection （14AA）， and has the advantages of rapid analysis， simple operation， strong specificity and high accuracy， making it suitable for the routine quality control of glycerol， acetic acid and sodium bisulfite in this preparation. This method provides a reliable analytical and testing tool for the quality assurance and safety control of compound amino acid injection （14AA） d","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"806-811"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352149/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414368","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":"[Innovative undergraduate teaching practice integrating MassWorks mass spectrometry analysis technology with gas chromatography-low resolution mass spectrometry].","authors":"Zhen-Xing Li, Yu'an Sun, Bin Li, Wen-Hao Yu, Wei-Min Ouyang, Ya-Chang Xu, Kuan Tian, Jian-Bo Zhao","doi":"10.3724/SP.J.1123.2025.11005","DOIUrl":"10.3724/SP.J.1123.2025.11005","url":null,"abstract":"<p><p>Mass spectrometry professionals are in short supply industry-wide. Undergraduate teaching has bottlenecks： limited instrumentation， weak qualitative skills and abstract theoretical concepts. We report an innovative pedagogy coupling conventional gas chromatography-mass spectrometry （GC-MS） with the MassWorks^TM software suite. A 14-component fragrance standard mixture was employed to design an experiment spanning the entire workflow separation， detection， exact-mass measurement， isotopic-pattern matching， molecular-formula assignment， structural elucidation. By exploiting the software's dual-calibration algorithms for exact-mass and isotopic-profile refinement， the mass accuracy and qualitative reliability of GC-low resolution MS data were dramatically enhanced. The practical results show that this method improves the quality accuracy of MS data by 100 times， controls the mass deviation within |Δ<i>m</i>|≤10 mDa， achieves an accuracy of over 98% in isotope spectra， and provides accurate and reliable qualitative results. The teaching effect is significant. Through the closed-loop training of theoretical analysis， software application， and practical verification， students' scientific research thinking， data analysis ability， and innovative ability to solve complex problems have been effectively improved. This provides a replicable and scalable effective paradigm for improving the quality of instrument analysis teaching under limited resource conditions.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"827-833"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352145/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414412","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 chiral micro-packed high performance liquid chromatography column with small-size silica gel coated with amylose tris（3，5-dimethylphenylcarbamate）].","authors":"Cheng-Gui Zhang, Yi-Xing Long, Heng Liu, Yin-Cui Song, Yun-Tao Liang, Li-Ming Yuan","doi":"10.3724/SP.J.1123.2025.07016","DOIUrl":"10.3724/SP.J.1123.2025.07016","url":null,"abstract":"&lt;p&gt;&lt;p&gt;The separation of chiral compounds using common dimension chiral chromatographic columns consumes a large of mobile phase and a long time. This is mainly due to the fact that the inner diameter of common chiral chromatographic column is usually 4.6 mm and the column length is 25 cm. The larger column volume requires more mobile phase to drive the sample through the separation process， and the longer column length increases the migration path of the sample within the column， resulting in an extended separation time. Moreover， the common dimension chiral column is filled more stationary phase which is usually expensive. The micro-packed column， due to their structural characteristics， with inner diameters typically controlled and a few millimeters and significantly shortened column lengths， show broad application prospects in improving separation efficiency， achieving miniaturization of separation instruments， and reducing the consumption of stationary and mobile phases. In this study， amylose tris（3，5-dimethylphenylcarbamate） （ADMPC） was used as the chiral selector. Amylose molecules have a helical structure， and the size of the helical cavity and the chiral environment can be regulated through substituent modification. The introduction of 3，5-dimethylphenylcarbamate groups can enhance the hydrophobic interaction， hydrogen bonding， and &lt;i&gt;π-π&lt;/i&gt; stacking between ADMPC and chiral compounds， thereby improving chiral recognition ability. Due to its excellent selectivity and wide applicability， it has become a research hotspot in the field of chiral separation. Two 10-millimeter-long micro-packed columns were prepared by coating ADMPC on silica gel particles with diameters of 500 nm and 1.7 μm， respectively， and were named ADMPC-1 （500 nm silica gel） and ADMPC-2 （1.7 μm silica gel）. On these two micro-packed columns， 23 and 20 racemates， respectively， including various types such as alcohols， esters， ketones， and acids， achieved good separation effects. Notably， there are certain differences in separation selectivity between these two micro-packed columns， showing a certain degree of complementarity. Moreover， these two micro-packed columns also exhibit this complementary property compared with the commercial Chiralpak AD-H chiral column. The most significant advantage of micro-packed columns is the short separation time， most compounds can be separated within 8 min， and many compounds can achieve baseline separation. Commercial chiral columns， due to their longer column lengths， usually require 15-30 min or even longer for sample retention time， and some compounds may not achieve baseline separation due to insufficient resolution. The shorter column length and optimized small size silica gel of micro-packed columns significantly reduce the retention time of samples and improve resolution， which is of great significance for high-throughput screening experiments （such as chiral compound screening in drug development）， and can significantly impro","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 7","pages":"795-805"},"PeriodicalIF":0.0,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13352144/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148414354","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}