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ANALYTICA CHIMICA ACTA · 2015 · IF 4.513

A reversed-phase/hydrophilic interaction mixed-mode C18-Diol stationary phase for multiple applications

Qing Wang,Mao Ye,Li Xu,Zhi-guo Shi

A mixed-mode chromatographic packing material, C18 and diol groups modified silica (C18-Diol), was prepared with controllable hydrophobicity and hydrophilicity . It demonstrated excellent aqueous compatibility and stability in aqueous mobile phase ; compared to the traditional C18 column, improved peak shape of basic analytes was also obtained. Additionally, it exhibited both reversed-phase liquid chromatographic (RPLC) and hydrophilic interaction chromatographic (HILIC) performance; the analyte separation scope was thus enlarged, demonstrated by simultaneous separation of twenty acids, bases and neutrals. More interestingly, a novel on-line two-dimensional liquid chromatography on the single column (2D-LC-1C) was established by modifying the high performance liquid chromatographic instrument only with the addition of an extra six-port two-position valve. The early co-eluted components of the extract of Lonicera japonica on the 1st-dimension (RPLC) were collected for the online re-injection to the 2nd-dimension (HILIC) by conveniently varying the mobile phase components. Six more peaks were obtained. The established system was simple, easy operation and low cost, which had advantages in analyzing complicated samples.

研究领域: 分析化学 · 药物分析 · 色谱技术
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Preparation of ionic gel-modified stationary phase for RPLC/HILIC/IC separation and its application in per aqueous liquid chromatography

Xiang Wang,Xingrui Wang,Hanqi Yang,Hanlin Zeng,Zhiqiang Xu,Wenhao Chen,Guangming Zhou,Jingdong Peng

In this study, we synthesized and employed an ionic gel-functionalized silica stationary phase for high-performance liquid chromatography. The successful fabrication of the stationary phase was confirmed through attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), zeta-potential measurements, and elemental analysis (EA). Comparative performance evaluation against a commercial column demonstrated the prepared column's effectiveness in the mixed mode of reversed-phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), and ion chromatography (IC). Moreover, the stationary phase exhibited exceptional retention repeatability in per aqueous liquid chromatography, showcasing its potential as an environmentally friendly analytical method. Mechanistic investigations unveiled multiple solute-stationary phase interactions, including π-π interactions, hydrogen bonding, and ion exchange. Finally, we applied the developed stationary phase for the precise detection of preservatives in carbonated beverages and jelly, achieving high levels of accuracy and recovery rates.

CAS / MDL: 97-90-5 121-44-8 78-67-1
研究领域: 分析化学 · 环境科学 · 食品科学
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JOURNAL OF CHROMATOGRAPHY A · 2019 · IF 3.858

Preparation of two ionic liquid bonded stationary phases and comparative evaluation under mixed-mode of reversed phase/ hydrophilic interaction/ ion exchange chromatography

Xiang Wang,Jingdong Peng,Huanjun Peng,Jun Chen,Hong Xian,Ranxi Ni,Shiyu Li,Dengying Long,Zhongying Zhang

The present work describes the preparation of two ionic liquid and carboxyl acid silane reagents via photo-initiated thiol-ene click chemistry that have been bonded to silica to afford two mixed-mode stationary phases (Sil-C4Im-C9Co and Sil-C9Im-C4Co). The two stationary phases provided satisfactory retention repeatability and efficiencies. The influence of acetonitrile content, salt concentration and pH of the mobile phase was investigated to clarify the retention properties of the prepared stationary phases. The results showed that the prepared Sil-C4Im-C9Co and Sil-C9Im-C4Co undergo multiple interactions with solutes under different chromatographic conditions. The retention mechanisms were further studied by the linear energy solvation relationship and Van’t Hoff plots. Finally, the stationary phases were employed to separate hydrophobic solutes (alkylbenzenes and polycyclic aromatic hydrocarbons) under reversed phase liquid chromatography (RPLC) mode, hydrophilic solutes (carboxylic acids, nucleosides and bases) under hydrophilic interaction liquid chromatography (HILIC) mode and inorganic anions under ion-exchange chromatography (IEC) mode, providing excellent performance and varying selectivity when compared with a commercial column. The bonding method in this work is feasible and the prepared stationary phases are promising when employed in RPLC/HILIC/IEC mixed-mode chromatography applications.

研究领域: 分析化学 · 材料科学
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Octadecylamine dendrimers modified silica for novel mixed-mode liquid chromatographic stationary phases

Honglin Yang,Bing Guo,Xuemei Dai,Meifang Liao,Jing Ou,Yaxin Yang,Lian Zhong,Yanyu Jiang,Jie Wen,Lujun Wang

Two novel octadecylamine dendritic stationary phases, called Sil-G1-AS and Sil-G2-AS, were innovatively prepared by grafting ethylenediamine and 1,4-butanediol diglycidyl ether (BDDE) onto silica surface, followed by octadecylamine (AS), and further used for mixed-mode chromatography (MMC). The prepared materials and intermediates were characterized using Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), contact angle analysis and thermogravimetric analysis (TGA). The chromatographic behavior of Sil-G1-AS and Sil-G2-AS columns was investigated using compounds of phenols, alkylbenzenes , nucleosides , polycyclic aromatic hydrocarbons (PAHs), vitamins, alkaloids, anilines, aromatic acids and flavonoids . The prepared stationary phases exhibited MMC behavior of reversed-phase liquid chromatography (RPLC), ion exchange chromatography (IEC) and hydrophilic interaction chromatography (HILIC) under different mobile phase conditions. Among them, Sil-G2-AS stationary phase has stronger hydrophilic properties and performs better chromatographic performance in HILIC, while Sil-G1-AS has stronger hydrophobicity . In addition, the stability of the two chromatographic columns was further investigated. These results demonstrated that Sil-G1-AS and Sil-G2-AS columns can provide multiple retention modes for the separation of a wide range of analytes with excellent stability.

CAS / MDL: 107-15-3
研究领域: 分析化学 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2018 · IF 3.716

Preparation and evaluation of a reversed-phase/hydrophilic interaction/ion-exchange mixed-mode chromatographic stationary phase functionalized with dopamine-based dendrimers

Di Zhou,Jing Zeng,Qifeng Fu,Die Gao,Kailian Zhang,Xiujun Ren,Kai Zhou,Zhining Xia,Lujun Wang

In this work, a novel dendritic stationary phase was synthesized by the repeated grafting of 1,4-butanediol diglycidyl ether (BDDE) and dopamine (DA) on the surface of silica for performing mixed-mode high-performance liquid chromatography (MHPLC). Elemental analysis (EA), thermogravimetric analysis (TGA) and Fourier transform infrared spectrometry (FT-IR) showed the successful preparation of the dendritic stationary phase. The prepared stationary phase showed the retention mechanisms of reversed-phase liquid chromatography (RPLC), hydrophilic interaction chromatography (HILIC) and ion-exchange chromatography (IEC) under different mobile phase conditions. In detail, alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs) and hydrophobic positional isomers were separated successfully in the RPLC mode. The baseline separation of nucleobases, nucleosides and flavonoids was achieved under HILIC mode, respectively. Meanwhile, some acidic and basic analytes were used to evaluate the IEC mode. The effects of different chromatographic conditions, such as acetonitrile content, salt concentration and pH in the mobile phase, on the different chromatographic modes were also investigated. In addition, the application of the mixed-mode dendritic stationary phase was demonstrated by the analysis of traditional Chinese medicine (TCM), including Carthamus tinctorius L. and Abelmoschus manihot (Linn.) Medicus. Interestingly, the stationary phase also has the ability for the capture and separation of boric acids. These meaningful applications confirmed that the mixed-mode dendritic stationary phase can be potentially applied in the analysis of complex samples.

CAS / MDL: 62-31-7
研究领域: 分析化学 · 材料科学
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Analytical Methods · 2021 ·Vol. 13 ·期 26 ·2989-2996 · IF 2.896

Qualitative and quantitative determination of trace aldehydes and ketones in food preservative propionic acid for quality improvement

Yiwen Cao,Shenjie Zhu,Lin Zhang,Qun Cui,Haiyan Wang

Aiming at the difficulty in qualitative and quantitative analysis of trace compositions in food preservative propionic acid, the trace compositions and the key components influencing the total aldehyde content in propionic acid were analyzed by gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography (HPLC) and gas chromatography (GC) in this paper. The results show that the food preservative propionic acid contains 18 trace compositions. The main compositions affecting the total aldehyde content in propionic acid are acetaldehyde, propionaldehyde, 1-cyclopropyl-1-propanone and 2-methyl-2-pentenal, which account for ∼90% of the total aldehyde content in propionic acid. The total aldehyde content in propionic acid can be quickly determined by iodometric titration. However, the impurity compositions, solution oxygen content and pH value of propionic acid may affect the stability of NaHSO3, which lead to a higher titration value of the aldehyde content. The total aldehyde contents in propionic acid determined by GC (148.535–337.890 mg L−1) and HPLC (157.730–335.780 mg L−1) are close and reliable with a relative deviation of 0.31–3.00%. The volatile low-carbon aldehydes and ketones including formaldehyde, acetaldehyde and acetone have a weak response and a high detection limit in GC. The derivation conditions of all aldehydes and ketones in propionic acid should affect the determination results of HPLC. It provides the basic data for quality improvement and ultra-deep purification of food-grade propionic acid.

研究领域: 食品科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Additional band broadening of peptides in the first size-exclusion chromatographic dimension of an automated stop-flow two-dimensional high performance liquid chromatography

Jucai Xu,Dongxiao Sun-Waterhouse,Chaoying Qiu,Mouming Zhao,Baoguo Sun,Lianzhu Lin,Guowan Su

The need to improve the peak capacity of liquid chromatography motivates the development of two-dimensional analysis systems. This paper presented a fully automated stop-flow two-dimensional liquid chromatography system with size exclusion chromatography followed by reversed phase liquid chromatography (SEC   ×   RPLC) to efficiently separate peptides. The effects of different stop-flow operational parameters (stop-flow time, peak parking position, number of stop-flow periods and column temperature) on band broadening in the first dimension (1 st D) SEC column were quantitatively evaluated by using commercial small proteins and peptides. Results showed that the effects of peak parking position and the number of stop-flow periods on band broadening were relatively small. Unlike stop-flow analysis of large molecules with a long running time, additional band broadening was evidently observed for small molecule analytes due to the relatively high effective diffusion coefficient ( D eff ). Therefore, shorter analysis time and lower 1 st D column temperature were suggested for analyzing small molecules. The stop-flow two-dimensional liquid chromatography (2D-LC) system was further tested on peanut peptides and an evidently improved resolution was observed for both stop-flow heart-cutting and comprehensive 2D-LC analysis (in spite of additional band broadening in SEC). The stop-flow SEC   ×   RPLC, especially heart-cutting analysis with shorter analysis time and higher 1 st D resolution for selected fractions, offers a promising approach for efficient analysis of complex samples.

研究领域: 分析化学 · 生物化学
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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Configuration of the ion exchange chromatography, hydrophilic interaction chromatography, and reversed-phase chromatography as off-line three-dimensional chromatography coupled with high-resolution quadrupole-Orbitrap mass spectrometry for the multicomponent characterization of Uncaria sessilifructus

Keyu Feng,Simiao Wang,Lifeng Han,Yuexin Qian,Huifang Li,Xue Li,Li Jia,Ying Hu,Huimin Wang,Meiyu Liu,Wandi Hu,Dean Guo,Wenzhi Yang

Herbs represent complex chemical systems involving various primary and secondary metabolites that are featured by large spans of acid-base property, polarity, molecular mass, and content, etc. , which thus poses great challenges to characterize the metabolites contained. Here, the combination of multiple-mechanism chromatography coupled with improved data-dependent-MS 2 acquisition (DDA-MS 2 ) is presented as a strategy to support the deep metabolites characterization. Targeting Uncaria sessilifructus , a reputable medicinal herb containing alkaloids and triterpenic acids (TAs) as the main pharmacologically bioactive ingredients, a three-dimensional liquid chromatography (3D-LC) system was established by integrating ion exchange chromatography, hydrophilic interaction chromatography, and reversed-phase chromatography (IEC-HILIC-RPC). The first-dimensional chromatography, configuring a PhenoSphere SCX column eluted by methanol/20 mM ammonium acetate-0.05% formic acid in water, could well fractionate the total extract into two fractions (unretained ingredients and alkaloids). The subsequent HILIC using an XAmide column and RPC by a CSH Phenyl-Hexyl column achieved the sufficient resolution of the total TAs and total alkaloids, respectively. A polarity-switching precursor ions list-including DDA approach by Q-Orbitrap-MS enabled the high-efficiency, coverage-enhanced identification of alkaloids and TAs. This 3D-LC/Q-Orbitrap-MS system was validated as precise (RSD < 5% for intra-day/inter-day precision), Up to 308 components were separated from U. sessilifructus , and 128 thereof (including 85 alkaloids, 29 TAs, and 14 others) were identified or tentatively characterized, exhibiting superiority over the conventional one-dimensional LC/MS. Conclusively, 3D-LC/MS in an off-line mode can facilitate the flexible configuration of multiple chromatography to accomplish the fit-for-purpose characterization of the metabolites from an herbal extract or a biosample.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 药学 · 质谱分析 · 中药学
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TALANTA · 2015 · IF 3.545

Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase

Qing Wang,Yao Long,Lin Yao,Li Xu,Zhi-Guo Shi,Lanying Xu

A mixed-mode chromatographic stationary phase , C18-DTT (dithiothreitol) silica (SiO 2 ) was prepared through “thiol-ene” click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen , guanine , tetrandrine and nicotinic acid) in the range of 1.82–3.72% and 0.85–1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids , alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons . It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase.

研究领域: 分析化学 · 材料科学
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BIOCHEMICAL ENGINEERING JOURNAL · 2025 · IF 3.8

An Ag+-assisted high-speed countercurrent chromatography and column chromatography for effective separating sciadonic acid from Torreya grandis oils

Meng Xianghe,Wang Shuyi,Lu Yuanchao,Nie Xiaohua,Ye Qin

Sciadonic acid (△5,11,14–20:3, SCA) is a rare versatile non-methylene-interrupted polyunsaturated fatty acid. To prepare high purity SCA from Torreya oils with 8.04 % purity, Ag + -assisted high-speed countercurrent chromatography (HSCCC) combined with urea complexation (UC) or argentation column chromatography (CC) was investigated. Results showed that n -hexane: acetonitrile (1:1, v/v) was suitable mobile phase for HSCCC, and SCA with purity of 23.74 % and recovery of 61.74 % (SCA purity>20 %) were obtained. When the Ag + addition was 0.50 %, one round of Ag + -HSCCC resulted in a recovery of SCA up to 95.38 % with purity around 21 %. It was believed that the enhanced performance originated from the reversible complexes between Ag + and C C in SCA through π-s * and d-π* bonds. Starting with low purity SCA of 8.04 %, HSCCC (23.74 %), UC (62.67 %), or Ag + -CC (60.41 % ) alone failed to produce SCA with high-purity (>90 %). However, Ag + -HSCCC combined with Ag + -UC or Ag + -CC yielded SCA with purities of 76.21 % and 97.74 %, and overall recovery of 21.38 % and 19.31 %, respectively. Thus, Ag + -HSCCC was an efficient method for the pre-enrichment of SCA, which could effectively facilitate coupling with UC, Ag + -CC or other PUFA purification techniques, resulted in significant improved purification performances.

研究领域: 植物化学 · 分离技术
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Analytical Methods · 2014 ·Vol. 6 ·期 7 ·2205-2214 · IF 1.938

Preparation, chromatographic evaluation and comparison of cystine- and cysteine-bonded stationary phases

Luan Xu,Tong Zhao,Xingmei Guan,Wanjin Tang,Xiaoyan Liu,Haixia Zhang

In this paper, cystine- and cysteine-bonded stationary phases were synthesized and characterized by UV spectroscopy, Fourier transform infrared spectroscopy and elemental analysis which proved the successful immobilization of cystine and cysteine on the silica support. Both the new stationary phases displayed mixed-mode behavior, hydrophilic interaction chromatography (HILIC) mode and reversed-phase liquid chromatography (RPLC) mode. Retention behaviors of polar compounds on the two stationary phases were studied under different mobile phases by varying their water content, pH and ionic strength. The separation of sulfanilamide and substituted benzoic acid compounds was demonstrated on the new phases.

研究领域: 分析化学 · 色谱技术 · 生物化学
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JOURNAL OF CHROMATOGRAPHY A · 2014 · IF 4.258

Experimental comparison of chiral metal-organic framework used as stationary phase in chromatography

Sheng-Ming Xie,Mei Zhang,Zhi-Xin Fei,Li-Ming Yuan

Chiral metal-organic frameworks (MOFs) are a new class of multifunctional material, which possess diverse structures and unusual properties such as high surface area, uniform and permanent cavities, as well as good chemical and thermal stability. Their chiral functionality makes them attractive as novel enantioselective adsorbents and stationary phases in separation science. In this paper, the experimental comparison of a chiral MOF [In 3 O(obb) 3 (HCO 2 )(H 2 O)] solvent used as a stationary phase was investigated in gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC). The potential relationship between the structure and components of chiral MOFs with their chiral recognition ability and selectivity are presented.

研究领域: 分析化学 · 材料科学
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