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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2025 · IF 3.8

Impact of silicon substrate on micro gas chromatographic column using ALD alumina as the stationary phase

Ma Shaojie,Zhu Yuchen,Li Wenbo,Chen Boxin,Zhao Bin,Feng Fei

Due to the high conformal films, atomic layer deposition (ALD) alumina has been used as a uniform stationary phase or support layer of stationary phase for micro gas chromatographic column. However, the severe tailing of chromatographic peaks appears when ALD alumina is used as the stationary phase. Recently, an H-diffusion model was proposed to explain the H accumulation phenomenon of ALD alumina films. Compared with the normal-resistance silicon substrates, the ALD alumina films based on low-resistance silicon substrates have fewer H impurities, which may further improve the tailing of chromatographic peaks and the theoretical number of plates. In this paper, a micro gas chromatographic column based on the low-resistance silicon (LR-μGCC) substrate (resistivity, 0.001–0.005 Ω·cm) using alumina deposited by atomic layer deposition as the stationary phase is reported. Compared with normal-resistance silicon substrates (resistivity, 1–10 Ω·cm), the micro gas chromatographic columns (μGCC) prepared on low-resistance silicon substrates have a higher separation performance. The test results showed that the LR-μGCC increased the theoretical plate number of alkane mixtures (n-hexane, n-octane, n-nonane, and n-decane) by 20.9%, 74.8%, 139.4%, and 55.4%, respectively, and reduced the tailing factor by 13.0%, 41.8%, 48.6%, and 49.1%, respectively. Graphical

研究领域: 分析化学 · 材料科学
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ELECTROPHORESIS · 2016 ·Vol. 37 ·期 10 ·1367-1375 · IF 2.482

Graphene oxide-SiO2 hybrid nanostructure as coating material for capillary electrochromatography

Qishu Qu,Han Xuan,Kehua Zhang,Yi Ding,Qin Xu

Graphene oxide (GO) has been considered as a promising stationary phase for chromatographic separation. However, the very strong adsorption of the analytes on the GO surface lead to the severe peak tailing, which in turn resulting in decreased separation performance. In this work, GO and silica nanoparticles hybrid nanostructures (GO/SiO 2 NPs@column) were coated onto the capillary inner wall by passing the mixture of GO and silica sol through the capillary column. The successful of coating of GO/SiO 2 NPs onto the capillary wall was confirmed by SEM and electroosmotic flow mobilities test. By partially covering the GO surface with silica nanoparticles, the peak tailing was decreased greatly while the unique high shape selectivity arises from the surface of remained GO was kept. Consequently, compared with the column modified with GO (GO@column), the column modified with GO and silica nanoparticles through layer-by-layer method (GO-SiO 2 NPs@column), or the column modified with silica nanoparticles (SiO 2 NPs@column), GO/SiO 2 NPs@column possessed highest resolutions. The GO/SiO 2 NPs@column was applied to separate egg white and both acidic and basic proteins as well as three glycoisoforms of ovalbumin were separated in a single run within 36 min. The intra-day, inter-day, and column-to-column reproducibilities were evaluated by calculating the RSDs of the retention of naphthalene and biphenyl in open-tubular capillary electrochromatography. The RSD values were found to be less than 7.1%.

CAS / MDL: 3179-76-8
研究领域: 分析化学 · 材料科学
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TALANTA · 2022 · IF 6.556

A guide of column selection for two-dimensional liquid chromatography method development of natural alkaloids

Yang Xu,Yanfang Liu,Han Zhou,Rong Wang,Dongping Yu,Zhimou Guo,Xinmiao Liang

Natural products , especially alkaloids, are one of the most valuable, potential drug leads in drug discovery. As an efficient tool for complex samples, two-dimensional liquid chromatography (2D-LC) has become a powerful means of analysis and separation of natural alkaloids. Method development of 2D-LC is of great importance because it helps to enhance the selectivity, resolution and peak capacity of a separation system. However, due to the diversity of the nature and subclasses of natural alkaloids, peak tailing occurs frequently, making alkaloid separation complicated and time-consuming. To conquer such difficulties, we proposed a guide for column selection and combination in 2D-LC so as to improve the alkaloid separation. Based on a comprehensive evaluation of applicability and orthogonality of several columns, this guide would provide a simple but clear starting point for column selection of 2D-LC method development. The evaluation included seven columns to involve most separation mechanisms reported in alkaloid separation, and 49 natural alkaloid standards of various subclasses and natures. Detailed studies of peak shapes of every column were carried out as well, providing useful references to better understand the peak tailing issues of some analytes on specific columns. Subsequently, a 2D-LC method was developed using our guide to isolate an alkaloid sample from U. rhynchophylla , generating symmetrical peaks and a high orthogonality of 80.3%. Further, this evaluation process would help to have a quick understanding when a new stationary phase is designed.

CAS / MDL: 540-69-2 64-18-6
研究领域: 分析化学 · 药学 · 天然产物化学
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JOURNAL OF CHROMATOGRAPHY A · 2020 · IF 4.049

Ultramicroporous metal-organic frameworks for capillary gas chromatographic separation

Sha-Sha Meng,Ze-Rong Tao,Wen-Qi Tang,Ting Han,Yan Du,Zhi-Yuan Gu

ABSTRACT Fine-tuning of the SiF 6 2− -containing metal-organic frameworks (SIFSIX) through the substitution of metal centers and ligands changed the apertures from 8.3 Å to 3.8 Å, resulting in ultramicropores and notably improving the separation performance of alkane isomers. Herein, we reported SIFSIX-1-Zn, SIFSIX-1-Cu and SIFSIX-3-Zn as representative stationary phases for capillary gas chromatography (GC). The capillary column coated with ultramicroporous SIFSIX-3-Zn efficiently separated the alkane isomers and benzene homologues, which outperformed SIFSIX-1-Zn and SIFSIX-1-Cu. This resulted from size matching between the window of the ultramicroporous SIFSIX-3-Zn and the analytes, which was also supported by McReynolds constants, column efficiency and peak tailing effect. It opened up a new avenue for ultramicroporous materials in the chromatography separation of isomers.

研究领域: 分析化学 · 材料科学 · 色谱学
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