TALANTA
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2021
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IF 6.057
Xi Lin,Chunsheng Xiao,Ling Ling,Liming Guo,Xinhua Guo
Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a widely used tool for the analysis of carbohydrates. However, the detection of carbohydrates by MALDI-TOF MS is often limited by the unsatisfactory ionization efficiency, instability and the matrix interference in low molecular weight region. Here, we demonstrate that a reactive matrix, 2-hydrazinoquinoline (2-HQ), can be used to detect neutral, sialic and low molecular weight carbohydrates sensitively both in the positive and negative ion mode. Since 2-HQ reacts efficiently with the reducing end of carbohydrate to form stable hydrazone , the ionization efficiency of derived carbohydrates is significantly enhanced. Using 2-HQ, the sensitivity for analyzing glycans has been improved 10-fold and 100-fold compared with those using 3-aminquinoline (3-AQ) and 2,5-dihydroxybenzoic acid (DHB) as matrix, respectively. Moreover, quantitative analysis of neutral, acidic and low molecular weight carbohydrates has been achieved because of the good reproducibility by using 2-HQ as matrix. As a result, up to 50 glycans in a single sample spot of human fresh serum without any prior purification and enrichment have been successfully detected. Therefore, 2-HQ as a new reactive matrix has shown great potentials in widespread applications for sensitive, selective, quantitative, high speed and high throughput analysis of carbohydrates in complex samples by MALDI-TOF MS.
研究领域:
分析化学
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质谱分析
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碳水化合物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2026
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IF 5.2
Xin Xin,Qi Zhang,Sujun Yan,Zilong Chen,Xinhai Zhu
Background Monosaccharides and disaccharides are central components of carbohydrate metabolism, and fluctuations in their abundances are closely associated with disease onset, progression, and diagnostic outcomes. However, accurate analysis of trace-level saccharides in complex biological matrices remains challenging due to their limited chromatographic retention, modest ionization efficiency, and limited MS/MS fragmentation. Derivatization has been widely explored to improve analytical performance in LC-MS-based saccharide analysis; nevertheless, further development of simple, sensitive, and broadly applicable strategies is desirable, particularly for small-volume and low-abundance biological samples. This work presents an efficient derivatization-LC-MS approach enabling ultrasensitive quantification of saccharides under microscale analytical conditions. Results A derivatization strategy based on 2-hydrazinyl-6-methoxy-1,3-benzothiazole (HMBT) was developed to enhance LC-MS analysis of monosaccharides and disaccharides. The mild reaction generated stable derivatives directly compatible with LC-MS. HMBT tagging significantly improved chromatographic retention and separation on conventional C18 columns and markedly enhanced ionization efficiency. The derivatives produced high-intensity precursor ions and a dominant, highly responsive product ion, enabling ultrasensitive MRM detection on a triple-quadrupole system. Using nine representative saccharides, the method achieved excellent quantitative linearity down to 10 pg·mL −1 . Application to mouse serum enabled the quantification of glucose at single-cell-equivalent levels, and spiked galactose showed a linear range of 0.05–100 ng·mL −1 . Importantly, the workflow enabled quantification of five endogenous saccharides in individual HeLa cells. Significance The HMBT derivatization workflow provides an ultrahigh-sensitivity LC-MS platform for saccharide analysis, enabling robust MRM-based quantification at pg·mL −1 levels. Its operational simplicity, minimal sample handling, and full compatibility with conventional LC-MS instrumentation facilitate practical implementation. The demonstrated applicability to true single-cell measurements highlights its potential for glycometabolic studies in microscale biological systems.
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF INORGANIC BIOCHEMISTRY
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2021
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IF 4.155
Rui-Xue Liu,Ru-Yi Luo,Meng-Ting Tang,Yan-Cheng Liu,Zhen-Feng Chen,Hong Liang
Based on the anticancer pharmacophore of anthrahydrazone and quinoline, a new quinolylanthrahydrazone ligand, 9-AQH (anthracene-9-quinolylhydrazone), was synthesized to further afford four metal complexes, [Co II (9-AQH)(NO 3 ) 2 (H 2 O)] ( 1 ), [Ni II (9-AQH) 2 (H 2 O) 2 ]·2NO 3 ( 2 ), [Cu I (9-AQH) 2 ]·NO 3 ( 3 ), [Zn II (9-AQH) 2 (NO 3 )]·NO 3 ( 4 ), determined by X-ray single crystal diffraction analysis. The reaction of Cu(NO 3 ) 2 with 9-AQH formed the stable and repeatable copper(I) complex 3 . In vitro screening demonstrated only 3 showed significant and broad-spectrum anticancer activity , indicating that Cu(I) played a key role in exerting the anticancer activity. In solution, Cu(I) was not naturally oxidized to Cu(II) suggested by 1 H-NMR (Nuclear Magnetic Resonance) and EPR (Electron Paramagnetic Resonance) analysis. The presence of 3 could also catalyze the H 2 O 2 system to give hydroxyl free radicals , suggested by further EPR and electrophoresis assay. At the cellular level, although no obvious Cu(II) signals were detected and the total ROS (Reactive Oxygen Species) scavenging in the tumor cells treated with 3 , the potential redox property between Cu(I)/Cu(II), as a key role, should not be denied for the significant anticancer activity of 3 , considering the much complicated circumstance and other reductive substances in cells. The anticancer mechanism of 3 on the most sensitive MGC-803 cells pointed to significant cell apoptosis through mitochondrial pathway, rather than cell cycle arrest . While the autophagy observed in tumor cells treated by 3 suggested its complicated anticancer mechanism, and whether there was an intrinsic correlation still needed to be further investigated.
研究领域:
无机化学
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药物化学
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癌症研究
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细胞生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）