ANALYST
·
2023
·Vol. 148
·期 14
·3392-3402
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IF 4.2
Danni Wang,Quanshou Feng,Yiting Luo,Weimin Wang,Yinghua Yan,Chuan-Fan Ding
In this work, titanium-rich hydrazide-linked porous organic polymers (hydrazide-POPs-Ti4+) were synthesized using hydrazine, 2,3-dihydroxyterephthalaldehyde (DHTA) and trimethyl 1,3,5-benzenetricarboxylate (TP) as the ligands. Hydrazide-POPs-Ti4+ combined with HILIC and IMAC can be used for simultaneous enrichment of glycopeptides and phosphopeptides. The detection limit of this protocol is 0.1 fmol μL−1 for glycopeptides and 0.005 fmol μL−1 for phosphopeptides, and the selectivities are 1 : 1000 and 1 : 2000 for glycopeptides and phosphopeptides, respectively. For practical bio-sample analysis, 201 glycopeptides associated with 129 glycoproteins and 26 phosphopeptides associated with 21 phosphoproteins were selectively captured from healthy human serum, and 186 glycopeptides associated with 117 glycoproteins and 60 phosphopeptides associated with 50 phosphoproteins were enriched in the serum of breast cancer patients. Gene Ontology analysis indicated that the identified glycoproteins and phosphoproteins were linked to breast cancer, including the binding of complement component C1q and low-density lipoprotein particles, protein oxidation and complement activation, suggesting that these connected pathways are probably engaged in the disease pathology of breast cancer.
研究领域:
分析化学
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生物化学
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分子生物学
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癌症研究
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DOI
PubMed
高影响因子
FITOTERAPIA
·
2024
·
IF 2.5
He Sun,Jia Lou,Bo-Xue Chen,Jia-Qi Huang,Qi-Long Wang,Shao-Fei Song,Zi-Yue Jia,Rong Miao,Shi-Yu Wang,Xue Li,Wen-Zhi Yang
Prunella vulgaris (PV) is a medicine and food homologous plant, but its quality evaluation seldom relies on the polysaccharides (PVPs). In this work, we established the multi-level fingerprinting and in vitro anti-inflammatory evaluation approaches to characterize and compare the polysaccharides of P. vulgaris collected from the major production regions in China. PVPs prepared from 22 batches of samples gave the content variation of 5.76–24.524 mg/g, but displayed high similarity in the molecular weight distribution. Hydrolyzed oligosaccharides with degrees of polymerization 2–14 were characterized with different numbers of pentose and hexose by HILIC-MS. The tested 22 batches of oligosaccharides exhibited visible differences in peak abundance, which failed to corelate to their production regions. All the PVPs contained Gal, Xyl, and Ara, as the main monosaccharides . Eleven batches among the tested PVPs showed the significant inhibitory effects on NO production on LPS-induced RAW264.7 cells at 10 μg/mL, but the exerted efficacy did not exhibit correlation with the production regions. Conclusively, we, for the first time, investigated the chemical features of PVPs at three levels, and assessed the chemical and anti-inflammatory variations among the different regions of P. vulgaris samples.
研究领域:
生药学
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分析化学
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药理学
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PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2026
·
IF 6.7
Xiaoqin Wang,Yujie Liao,Xiaoxiao Guo,Daohang Xing,Xiang Chen,Qian Wang,Linjuan Huang,Zhongfu Wang
Bovine lactoferrin (bLf) is an essential additive in infant formula, with its bioactivity closely related to N-glycosylation. Currently, the production cost of lactoferrin remains high. This study compared eight ion-exchange resins and identified DoWex and 732 as optimal for bLf purification. Yields reached 4.46% for DoWex and 5.25% for 732, with purities exceeding 85% for both resins. Isomer-specific N-glycan analysis using HILIC-MS/MS revealed 58 distinct N-glycans in mature bLf, including 28 neutral and 30 acidic glycans, with the acidic N-glycans predominantly modified by α2,6-linked Neu5Ac. The bLf prepared by 732 resin shared >97% of the neutral and >93% of the acidic glycans with that of DoWex. Notably, the price of 732 resin is only one-18th that of DoWex, representing a significant reduction in production costs and making it promising in future large-scale manufacturing. This work facilitates efficient lactoferrin production and provides further studies on the relationships between glycans and their functions.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Jinlin He,Luying Shen,Dunming Xu,Ting Sun,Yan Chen,Jinsheng Hu,Yan Ji,Lijuan Yan
First demonstration of C18-column HILIC-like separation for aminoglycosides. • Hydrophilic retention via water layer & vicinal silanols on base-deactivated silica. • Tandem WCX-C18 SPE protocol developed for effective matrix cleanup. • Robust, MS-compatible, practical monitoring of aminoglycoside residues in foods. An LC–MS/MS method was developed for the simultaneous determination of 16 aminoglycosides (AGs) in pork, chicken, milk, and eggs using a conventional Hypersil base-deactivated silica (BDS) C 18 column operated under HILIC-like conditions. Unlike typical C 18 -based methods that rely on ion-pairing reagents in the LC mobile phase, separation was achieved with an ion-pair-free mobile phase consisting only of 0.1% formic acid and acetonitrile under gradient elution. Column comparison, aqueous-fraction experiments, and SRM 870 probe testing indicated a mixed retention mechanism involving hydrophilic partitioning into a water-enriched interfacial layer and reversible interactions with accessible residual silanol sites. Because the method prioritizes MS compatibility and reproducible multi-residue quantification, compound-specific MRM transitions and matrix-matched calibration were used to ensure selectivity and quantitative reliability. The method showed good linearity (R² > 0.99), satisfactory accuracy (71.2–99.8%) with reported standard deviations, acceptable precision (CV ≤ 11.3%), and low detection limits (LODs 3–15 μg/kg; LOQs 10–50 μg/kg). Overall, this work demonstrates that a conventional C 18 column can exhibit pronounced hydrophilic selectivity under high-organic conditions, offering a practical, MS-friendly alternative for aminoglycoside residue analysis and informing future stationary-phase development for hydrophilic separations.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2013
·
IF 4.612
Qianying Sheng,Yanxiong Ke,Kuiyong Li,Dongping Yu,Xinmiao Liang
A hydrophilic interaction liquid chromatography (HILIC) stationary phase of cellulose-coated silica was synthesized as a novel saccharide separation material. The material, prepared with a method based on ionic interaction, was demonstrated to be efficient for immobilization of saccharides on silica supports. The method is more efficient than traditional immobilized saccharide stationary phase synthesis methods. It was evolved from a method using anion exchanger microparticles agglomerated onto macroparticles of cation exchangers to produce anion exchangers. Cationic cellulose, which has a large number of hydroxyl groups, was immobilized on sulfonated silica. The cellulose-coated stationary phase we designed used strong hydrogen bonding between cellulose hydroxyl and carbohydrate compounds for HILIC retention and separation. The stationary phase was successfully used to separate the samples of polar compounds and the complex samples of oligosaccharides, and demonstrated good reproducibility and stability. The material exhibited good separation selectivity for carbohydrates and ability to enrich glycosylated peptides. The method described here is easy to achieve, environmentally safe and innovative than other methods. It also has extensive application possibilities to separate other categories polar compounds.
研究领域:
分析化学
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色谱学
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材料科学
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PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2024
·
IF 7.7
Shuangyu Shao,Xiali Si,Yingtao Zhang,Jun Li,Pengfei Tu,Qingying Zhang
Quality analysis of edible mushrooms based on polysaccharides is generally difficult due to their complicated structures and hard separation. Here, multiple fingerprint analysis of polysaccharides based on chromatographic and spectrometric techniques were developed, and then applied in comparative analysis of Auricularia heimuer (AH), Auricularia cornea (AC), Auricularia cornea ʻYu Muerʼ (ACY) and Tremella fuciformis (TF). Firstly, polysaccharides were obtained with the molecular weights between 1.783 × 10 6 and 6.774 × 10 6 Da. Then, complete hydrolysis by TFA and enzyme digestion by cellulase were employed and subsequently analyzed by HPLC-UV, GC–MS, HILIC-HPLC-ELSD and HILIC-HPLC-ESI − -HCD-MS/MS, and ATR-FT-IR were used to characterize the functional groups of intact polysaccharides. By chemometric analysis, differential markers of d -xyl, l -fuc, l -arb, d -glc, disaccharide and hexasaccharide were selected, and AC and ACY were proved to be same species from the viewpoint of polysaccharides firstly. Furthermore, the structures of oligomers with DPs of 2–8 and →4)- β - d -Glc p -(1→ unit with different contents were inferred by combinatory analysis of ESI − -MS/MS, glycosidic linkage, monosaccharide compositions and functional groups. In conclusion, the combinatory method of multiple fingerprint and pattern recognition is powerful not only for structural elucidation of polysaccharides, but also for quality analysis and species differentiation of edible mushrooms from the perspective of biological polysaccharides.
研究领域:
食品科学
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分析化学
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真菌学
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生物化学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Irshad Hussain,Liu Shijiang,Nadeem Muhammad,Qamar Subhani,Ni Chengzhu,Umar Arif,Zhuo Yanhong,Zhu Yan
For reducing operational complexity and expenses in HPLC laboratories, the development of versatile mixed-mode stationary phases into a single platform as an alternative to using two or even three single-mode columns are in high demand. PAMAM dendrimers, characterized by a tunable multifunctional globular structure, have attracted considerable attention for the development of stationary phases. This study, for the first time, reports the synthesis of a mixed-mode stationary phase using G 2.0 PAMAM (mixed-core). The synthetic protocol involved three steps: (i) synthesis of conventional EDA-core dendrimer up to generation 1.5; (ii) aminolysis of resulting G 1.5 PAMAM with 1,8-diaminooctane (1,8-DAO) to obtain mixed-core G 2.0 PAMAM having aliphatic C8 groups; and (iii) its grafting to silica base followed by quaternization using glycidol. The synthesis and fabrication of this stationary phase was validated through NMR, FTIR, BET, TGA, zeta potential, and elemental analysis. The retention mechanism of the stationary phase was investigated by varying the chromatographic conditions and quantum chemistry calculations. The successful separation of a wide range of substances, including alkylbenzenes, polycyclic aromatic hydrocarbons, phenols, nucleosides and bases, organic acids, and inorganic anions on the newly developed column not only revealed its versatility for RPLC/HILIC/IEC mixed-mode chromatography, but also showed certain superiority to commercial columns. Moreover, the column exhibited excellent compatibility to 100% aqueous mobile phase–a step towards green chemistry principles for HPLC separations. The results implied that the proposed stationary phase holds significant prospects for separation of other classes of compounds, particularly the ones with certain degree of polarity.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yang Zhao,Yufang Ming,Yang Yang,Changyu Cai,Yujie Bi,Qing Fu,Yanxiong Ke
In this work, a chromatographic method for the separation of carbohydrates was proposed. Tris-(hydroxymethyl)-amine (TRIS) functionalized silica-based hydrophilic interaction liquid chromatography (HILIC) stationary was synthesized. The dynamically absorbed borate layer is generated by using borate buffer as a polar modifier due to the complexation of borate with TRIS ligand in the stationary phase. The chromatographic systems were analyzed by the linear solvation energy relationship model. The calculated system constants revealed the enhancement of anionic exchange by the addition of borate in the mobile phase system. In addition, ligand exchange is critical for the retention and elution order of sugars and sugar alcohols. Carbohydrates displayed prolonged retention with different selectivity profiles relating to their complexation coefficients with borate. Experiment results showed that the effect of borate in this chromatographic system was stable within the range of pH 3–7 and borate concentration of 5–15 mM. This work provides a complementary solution for the separation of carbohydrates. It can also be extended to the separation of glycosides.
研究领域:
分析化学
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色谱学
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碳水化合物化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2018
·
IF 3.716
Xingyun Zhao,Shengju Liu,Jiaxi Peng,Xin Li,Huan Niu,Hongyan Zhang,Li Wang,Ren’an Wu
A new hydrothermal carbon was prepared by a “one-pot” hydrothermal transformation of β-cyclodextrin on silica microspheres (noted as [email protected] microspheres), which was featuring as a new stationary phase for the hydrophilic interaction liquid chromatography (HILIC). The synthesized [email protected] possessed polar groups of hydroxyl, carbonyl and carboxyl groups arising from the carbonization transformation of β-cyclodextrin. As demonstrating great hydrophilicity, the [email protected] was applied as an excellent HILIC stationary phase for the separation of polar compounds including phenols and the endocrine disrupting chemicals (EDCs). In comparison with commercial available HILIC stationary phases, the separation performance of the [email protected] stationary phase was superior in the separation of phenols and EDCs. The mild hydrothermal carbon transformation of the β-cyclodextrin on the silica microspheres in the “one-pot” manner would represent a new and simple approach to prepare a new class of saccharide-derived stationary phases by using saccharides as precursors.
研究领域:
分析化学
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材料科学
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环境科学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Chao-Ping Hou,Ke Huang,Qiang Wang,Jin-Lan Yang,Hui-Bing Chen,Ying-Xia Zhang,Qi Liu,Zhi-Guang Li,Hui-Qing Li,Xu-Feng Wang
Tetrodotoxin (TTX), one of the most potent neurotoxins, poses a significant threat to consumer health. This study presents an advanced analytical method combining ion-paired reagent-assisted dispersive solid-phase extraction (ion-paired-dSPE) with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS), for the quantification of TTX residues in puffer fish. Edible tissue samples were extracted twice using a 1 % formic acid–methanol solution and purified via optimized ion-paired-dSPE procedures. TTX adsorbed onto the magnetic nano-adsorbents was subsequently eluted with an acetonitrile–water–formic acid solution (60:40:1, v/v/v). Detection was achieved through electrospray ionization in positive mode, with quantification performed in multiple reaction monitoring (MRM) mode. Correlation coefficients ( r ) in matrix-matched external standard curves ranged from 0.9995 to 0.9997. The limits of detection (LOD) and quantification (LOQ) in puffer fish tissues were 0.1 μg/kg and 0.3 μg/kg, respectively. Spiked recoveries at three concentrations in negative tissue samples ranged from 73.4 % to 87.5 %, with precision under 10.6 %. The method was validated in accordance with 2002/657/EC guidelines and successfully applied to TTX detection in cultured puffer fish samples.
研究领域:
食品科学
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分析化学
·
毒理学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Tiantian Si,Xiao Song,Licheng Wang,Yong Guo,Xiaojing Liang,Shuai Wang
A hydrophobically associating polyacrylamide (HAPM)-coated silica packing (HAPM@silica) as a novel stationary phase was synthesized by a simple thermal immobilization to separate multiple polar compounds for the first time. The successful immobilization of HAPM on the silica support was confirmed by elemental analysis, scanning electron microscopy (SEM) and the Brunauer–Emmett–Teller (BET). The thickness of HAPM coating is crucial and the one-layer HAPM@silica stationary phase was demonstrated the highest separation efficiency. Compared with the bare silica and amino modified silica, the new stationary phase showed better separation performance for multiple polar compounds such as bases, alkaloids, carbohydrates and amino acid compounds under the experimental conditions. The chromatographic behaviors were evaluated by investigating the effects of acetonitrile content, water content, mobile phase pH on separation. A typical hydrophilic interaction liquid chromatography (HILIC) retention feature of HAPM based column was observed at the low percentage of water content. The packing material also showed excellent chromatographic repeatability with intraday RSDs of the retention time of five bases less than 0.46% ( n = 10) and interday RSDs less than 1.45% ( n = 5). In summary, the new chromatographic material can be used for a feasible option for analysis of polar compounds.
研究领域:
分析化学
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色谱学
·
材料科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Tingting Liang,Shun Liu,Fang Wang,Jiamei Gu,Yang Lu,Weike Chen,Cunyu Li,Yunfeng Zheng,Guoping Peng
A specific, sensitive, rapid, precise, and reliable UPLC–MS/MS-based method was designed for the first time for the simultaneous determination of 1-deoxynojirimycin (DNJ) and N-methyl-1-deoxynojirimycin (N-CH 3 -DNJ) in rat plasma. Miglitol was served as the internal standard (IS). An MN-NUCLEODUR HILIC column was assessed to separate the two compounds by isocratic elution using acetonitrile : water with 0.05% formic acid and 6.5 mM ammonium acetate (72:28, v/v) at a flow rate of 0.4 mL/min. A triple quadrupole mass spectrometer was operated in the positive ionization mode using multiple reaction monitoring (MRM), and it was employed to determine transitions of m / z 164.1 → 110.1, 178.1 → 100.1, and 208.1 → 146.1 for DNJ, N-CH 3 -DNJ, and IS, respectively. The method of the two constituents was validated and the results were acceptable. The absolute bioavailability of DNJ and N-CH 3 -DNJ in rats was 50 ± 9% and 62 ± 24%, respectively. The method was then successfully used for the first time to study the pharmacokinetic behavior and absolute bioavailability of DNJ and N-CH 3 -DNJ in rats after intravenous (10 mg/kg) and oral administration (80 mg/kg). The results of this study might provide more information on preclinical pharmacokinetics and a solid basis for assessing the clinical efficacy of DNJ and N-CH 3 -DNJ.
研究领域:
药理学
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分析化学
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药学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）