JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
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2018
·
IF 0.827
Ting Qiao,Li-yun Ma,Xiaoling Wang,Zhi-Guo Shi
In the present study, the flow-through silica, featured with hierarchical pores, i.e., tunable mesopores and penetrable macropores, was attempted as the chromatographic stationary phase matrix to immobilize gold nanoparticles (AuNPs). It was first modified by mercapto groups (named as SiO2-SH), and then by AuNPs (named as SiO2-S-Au). Thanks to the characteristic macropores, the column backpressure of SiO2-S-Au was comparable to SiO2-SH, which effectively overcame the difficulty of high column backpressure upon the nanoparticles were introduced to the chromatographic matrix. Both the reversed-phase and hydrophilic interaction liquid chromatographic performance were observed on these two columns but with different selectivities. Hydrophobic, hydrophilic, hydrogen bond and electrostatic interactions between the SiO2-S-Au stationary phase and analytes could contribute to the retention. The SiO2-S-Au column showed excellent aqueous compatibility by “Stop-flow” test with the relative standard deviations (RSD) of analyte’s k (capacity factor) values from 0.59% to 2.88%. The reproducibility of SiO2-S-Au was acceptable with RSDs of analyte’s k values in the range of 3.13%-5.03%. In addition, compared with the SiO2-SH column, the SiO2-S-Au column had better separation performance and selectivity. The results demonstrated that the flow-through silica was a promising matrix for nanoparticles with low backpressure and different selectivities.
研究领域:
分析化学
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材料科学
✓ 已验证
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2025
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IF 6
Xiaoqian Yuan,Yuchen Cui,Yaqin Nan,Ruijun Tang,Xinru Wang,Yanmei Xu,Xinghua Jin,Yiwen Wang,Ding Cheng,Youxin Li
Background Cyclodextrins (CDs) and their derivatives have been widely used as chiral selectors in HPLC. However, many derivatized CDs lack specificity for certain drugs and often exhibit limited resolution. Furthermore, their synthesis typically involves complex multi-step procedures, hindering scalability and cost-efficiency. To overcome these limitations, this study aims to develop a simple and scalable boric acid-modified β-cyclodextrin polymer (BA-β-CDP), targeting chiral substances with O/N atoms in chiral and/or adjacent carbons. Results BA-β-CDP was synthesized on a large scale using inexpensive reagents and a random substitution strategy, avoiding tedious protection-purification steps. Structural and chromatographic compatibility was confirmed by nine characterization techniques. In HPLC using the chiral mobile-phase additive (CMPA) method, BA-β-CDP enabled the efficient separation of 25 racemates. Among them, 24 achieved complete or baseline separation, and 10 exhibited resolution (Rs) values > 10. Typical cases included bisoprolol (Rs = 48.19), propranolol (Rs = 45.50), chlorpheniramine (Rs = 38.36), and metoprolol (Rs = 20.26). Additionally, the material demonstrated excellent batch-to-batch reproducibility, recyclability, and reusability. Significance and novelty This work presents a practical and cost-effective chiral selector. The synergistic mechanism offers strong and specific recognition toward chiral substances with O/N atoms in chiral and/or adjacent carbons. This approach represents a novel strategy for efficient and economical HPLC-based enantioseparation using widely accessible materials and methods.
研究领域:
分析化学
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药物化学
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手性技术
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分子识别
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药剂学
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有机合成
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 10
·e70136
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IF 1.7
Yiyao Zhang,Guangyun Zhang,Fen Yang,Zhikang Zou
Hemoglobin A 1c (HbA 1c ) plays a role in the diagnosis and assessment of glycemic control in patients with diabetes. However, few studies have focused on the preparation methods and analytical performance evaluation of different formulations of mobile-phase buffers for HbA 1c assays. In this study, mobile-phase buffers of new formulations were prepared for the measurement of HbA 1c . Following the Clinical and Laboratory Standards Institute (CLSI) guidelines, the analytical performance of newly developed mobile-phase buffers was evaluated. The CVs of the intra- and inter-assay precision were less than 0.94%, the RDs of accuracy were less than ± 3.00%, and the carryover was 0.00%. The measured HbA 1c values were linear from 4.50% to 16.80% (26.00–160.00 mmol/mol). A comparison of newly developed and commercial mobile-phase buffers revealed that the Pearson regression equation was Y = 0.9862 x + 0.0888 ( R 2 = 0.9990), and the Bland–Altman mean difference between the two mobile-phase buffers was −0.02833% (95% CI: −0.1853% to 0.1278%). The chromatography column had a lifetime of over 7000 tests. The reference interval was 4.30%–6.30% (23.00–45.00 mmol/mol). Stability was acceptable within 24 months. The newly developed mobile-phase buffers demonstrated good analytical performance (i.e., precision, linearity, accuracy, carryover, reference interval, the number of chromatography column runs, and stability).
研究领域:
临床化学
·
糖尿病诊断
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分析方法验证
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色谱分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2024
·Vol. 47
·期 17
·2400462
·
IF 2.8
Yang Yang,Yuexin Li,Yang Zhao,Changyu Cai,Xinmiao Liang,Yanxiong Ke
In this work, monodisperse organosilane hybrid polymer microspheres with a particle size of about 5 µm were synthesized using seed swelling polymerization. The organosilicon reagent methacryloxypropyltrimethoxysilane was introduced into the polymer framework as a copolymerization monomer, and the crosslinking degree of the microspheres was improved by the hydrolysis-condensation reaction of siloxanes. The synthesized hybrid microspheres have good mechanical strength as well as low swelling, with swelling propensity values of 0.167 and 0.348 in methanol and acetonitrile, respectively. Hybrid microspheres modified with cysteine have a hydrophilic interaction chromatography/reversed-phase liquid chromatography mixed-mode retention mechanism. Compared to the commercial cysteine-modified silica column, the synthesized stationary phase has higher separation selectivity for partially acidic or basic samples and better basic resistance for use under high pH mobile phase conditions (at least 10).
研究领域:
分析化学
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材料科学
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色谱学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2023
·
IF 6.1
Qinsheng Chen,Qinwei Lu,Lianglong Zhang,Chenhan Zhang,Jingxian Zhang,Yu Gu,Qingxia Huang,Huiru Tang
Consistent retention time ( t R ) of metabolites is vital for identification in metabolomic analysis with ultrahigh-performance liquid-chromatography (UPLC). To minimize inter-experimental t R variations from the reversed-phase UPLC-MS, we developed an endo genous r etention- i ndex (endoRI) using in-sample straight-chain acylcarnitines with different chain-length ( L C , C0–C26) without additives. The endoRI-corrections reduced the t R variations caused by the combined changes of mobile phases , gradients, flow-rates, elution time, columns and temperature from up to 5.1 min–0.2 min for most metabolites in a model metabolome consisting of 91 metabolites and multiple biological matrices including human serum, plasma, fecal, urine, A549 cells and rabbit liver extracts. The endoRI-corrections also reduced the inter-batch and inter-platform t R variations from 1.5 min to 0.15 min for 95 % of detected features in the above biological samples. We further established a quantitative model between t R and L C for predicting t R values of acylcarnitines when absent in samples. This makes it possible to compare metabolites’ t R from different t R databases and the UPLC-based metabolomic data from different batches.
研究领域:
分析化学
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代谢组学
·
生物化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）