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JOURNAL OF CHROMATOGRAPHY A · 2016 · IF 3.926

Chemometrics-assisted high performance liquid chromatography-diode array detection strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for beverage analysis

Xiao-Li Yin,Hai-Long Wu,Hui-Wen Gu,Yong Hu,Li Wang,Hui Xia,Shou-Xia Xiang,Ru-Qin Yu

This work reports a chemometrics-assisted high performance liquid chromatography-diode array detection (HPLC-DAD) strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for the rapid simultaneous determination of six synthetic colorants in five kinds of beverages with little sample pretreatment. The investigation was performed using two types of LC columns under the same elution conditions. Although analytes using different columns have different co-elution patterns that appear more seriously in complex backgrounds, all colorants were properly resolved by alternating trilinear decomposition (ATLD) method and accurate chromatographic elution profiles, spectral profiles as well as relative concentrations were obtained. The results were confirmed by those obtained from traditional HPLC-UV method at a particular wavelength and the results of both methods were consistent with each other. All results demonstrated that the proposed chemometrics-assisted HPLC-DAD method is accurate, economical and universal, and can be promisingly applied to solve varying interfering patterns from different chromatographic columns and sample matrices for the analysis of complex food samples.

研究领域: 分析化学 · 食品科学
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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Separation performance of the copolymer and homopolymer of aliphatic polycarbonate diols as the stationary phases for capillary gas chromatography

Yingying Shi,Meiling Qi

This work presents the investigation of two aliphatic polycarbonate diols (CAPC and HAPC) as the stationary phases for capillary gas chromatography (GC). The CAPC and HAPC capillary columns showed moderate polarity and high column efficiency of 3704 – 4545 plates/m measured by n-octanol and naphthalene at 120 °C. It was found that despite their similar chemical compositions, CAPC and HAPC differ largely in their selectivity towards the isomers of alkanes, methylpyridines and xylenes. As demonstrated, the CAPC column exhibits advantageous comprehensive performance over the HAPC column and the commercial PEG column. Particularly, the CAPC column exhibits higher resolving performance towards the isomers indicated above and the Grob mixture than the HAPC column. Also, it shows distinct advantages over the PEG column in separating the Grob mixture, the isomers of diethylbenzenes and cymenes, and practical analysis of chemical products and the essential oil from the leaves of Rhododendron dauricum L. Additionally, the CAPC column has excellent repeatability and reproducibility on analyte retention times with the relative standard deviation (RSD) values in the range of 0.05% – 0.08% for run-to-run, 0.12% – 0.19% for day-to-day and 2.6% – 4.9% for column-to-column, respectively. Its applications to purity test of chemical products and GC–MS analysis of the essential oil demonstrate its promising future for practical GC analyses.

研究领域: 分析化学 · 色谱学
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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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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

A singular chromatographic column breakthrough: Achieving full polarity range separations with the epoxy propanol molecular cage bonded silica stationary phase

Litao Wang,Zhen Li,Ying Wang,Niannian Li,Dekuan Hu,Wei Wu,Jin xia Hu,Dong Pei,Mei Lv

The epoxy propanol molecular cage bonded silica stationary phase, RCC3-GLD@silica, synthesized through the ring-opening reaction of secondary amine with epoxy propanol using RCC3-R as the scaffold unit, was successfully prepared as confirmed by infrared spectroscopy, thermogravimetric analysis, and nitrogen adsorption-desorption characterization. This stationary phase demonstrated excellent separation performance in both reversed-phase and hydrophilic chromatography modes, effectively separating a wide variety of compounds including alkylbenzenes, polycyclic aromatic hydrocarbons, phenols, anilines, sulfonamides, nucleosides, amino acids, sugars, and acids. The development of RCC3-GLD@silica benefits from the synergistic effects of its hydrophobic and hydrophilic actions, as evidenced by the U-shaped characteristic of the retention factor for nucleoside compounds with changes in the aqueous content of the mobile phase, further confirming the simultaneous presence of reversed-phase and hydrophilic chromatography mechanisms. Not only did this stationary phase successfully separate 33 compounds in reversed-phase chromatography mode, but it also separated 54 compounds in hydrophilic interaction chromatography mode, showcasing its broad separation capability from weakly polar to strongly polar compounds on a single chromatographic column. This indicates a wide application prospect in the field of chromatographic analysis.

CAS / MDL: 106-89-8
研究领域: 分析化学 · 材料科学
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ANALYTICA CHIMICA ACTA · 2018 · IF 5.123

Selectivity of hexaphenylbenzene-based hydrocarbon stationary phase with propeller-like conformation for aromatic and aliphatic isomers

Yinhui Yang,Zhengfeng Chang,Xiaohong Yang,Meiling Qi,Jinliang Wang

Herein we report a propeller-like hexaphenylbenzene-based hydrocarbon material (denoted as BT) as the stationary phase for capillary gas chromatography (GC). The statically-coated BT capillary column showed a high column efficiency of 4340 plates m −1 and weak polarity. Owing to its unique conformation, π-electron toroidal delocalization and intrinsic microporosity , the BT stationary phase exhibited interesting selectivity for aromatic compounds over alkanes. Compared with the graphene (G) column, the BT column showed much prolonged retention and high selectivity for aromatic isomers, especially methylnaphthalenes , dimethylnaphthalenes and phenanthrene/anthracene, mainly because of its propeller-like conformation with rich intercalation effects. Moreover, it exhibited good column repeatability (intra-day, inter-day) and reproducibility (between-column) with RSD values on the retention times less than 0.08% for intra-day, 0.32% for inter-day and 3.8% for between-column, respectively. Also, it showed good potential for determination of minor isomer impurities in real samples. To the best of our knowledge, this work presents the first example of employing an neat aromatic hydrocarbon material as the GC stationary phase with high selectivity for analytes of a wide ranging polarity.

研究领域: 分析化学 · 材料科学
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NEW JOURNAL OF CHEMISTRY · 2020 ·Vol. 44 ·期 25 ·10621-10627 · IF 3.288

A novel column fabrication approach for capillary gas chromatography via a cross-linked organogel network with high stability and inertness

Xue Xiong,Meiling Qi

This work presents a novel column fabrication approach for capillary gas chromatography (CGC) through the condensation reaction of a hydroxyl-terminated polymer with a cross-linker inside a capillary column. In this work, polypropylene glycol (PPG 4000) and tris[3-(trimethoxysilyl)propyl]isocyanurate (ICS) were employed to fabricate the PPG-gel capillary column for GC analyses. Inside the column, a 3D cross-linked organogel network forms on the capillary inner surface by condensation of PPG 4000 with ICS under the given mild conditions. As a result, the PPG-gel column exhibited moderate polarity and showed distinctly advantageous resolving performance and inertness for carboxylic acids over the PPG column by the conventional static coating method. Also, it achieved high-resolution separations of the isomer mixtures of alkanes, alkylbenzenes and halobenzenes. Moreover, the PPG-gel column exhibited dramatically improved solvent stability because of its cross-linked organogel network. The organogel column displayed excellent column repeatability and reproducibility with the RSD% values in the range of 0.01–0.04% for run-to-run, 0.71–0.84% for day-to-day and 2.4–3.1% for column-to-column. The proposed organogel approach is facile and applicable to other analogous materials and has a promising future for wide applications.

研究领域: 分析化学 · 材料科学
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CHINESE JOURNAL OF ANALYTICAL CHEMISTRY · 2019 · IF 0.931

High Performance Micro Gas Chromatography Column Using Mesoporous Silica as Stationary Phase

Xue-Lei YANG,Bin ZHAO,Fei FENG,Hai-Mei ZHOU,Heng YANG,Xin-Xin LI

A semi-packed micro gas chromatography (μGC) column embedded micro-elliptical pillars was fabricated based on micro- electro-mechanical system (MEMS) technique. The mesoporous silica (MS) film with 2-nm pore size and large specific surface area was coated on the inner surface of the μGC column as stationary phase. A baseline separation of alkanes (C5–C10) was realized by the μGC column which used MS as stationary phase, and the resolution of pentane and solvent (impurity) was as large as 3.6. Compared with the μGC column which used polydimethylsiloxane (PDMS) as stationary phase under the same injection volume, the number of theoretical plates of octane had a 46% increase and reached up to 14458 plates. Meanwhile, the peak area of nonane was increased by 349.8%.

CAS / MDL: 78-10-4 70131-67-8
研究领域: 分析化学 · 材料科学 · 微纳制造
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JOURNAL OF CHROMATOGRAPHY A · 2018 · IF 3.716

Pore size effect of mesoporous silica stationary phase on the separation performance of microfabricated gas chromatography columns

Lei Hou,Fei Feng,Wenbin You,Pengcheng Xu,Fan Luo,Bowen Tian,Haimei Zhou,Xinxin Li

Microfabricated semi-packed gas chromatography (GC) columns coated with two kinds of mesoporous silica (MS) stationary phase have been explored and compared in this paper. The micro GC (μGC) columns are fabricated by microelectromechanical system (MEMS) technique. MSs with pore size of 2 and 5 nm are prepared using two different soft-templates and deposited on the inner surface of the μGC columns by dip-coating. For the first time, the influence of pore size of MS stationary phase on the separation performance in a μGC column has been investigated. As demonstrated, the mixtures of light alkanes (C1–C4) or heavy alkanes (C5–C10) can be well separated in both columns, where the separation resolution is always higher than 1.25 except for C1–C2 and C5–C6. Considering the pore size effect on the separation performance, it is shown that analytes, especially those with bigger size, display longer retention time in the column with larger pore size. For C10, the retention time in 5 nm-MS column is 200% longer than that in 2 nm-MS one.

CAS / MDL: 78-10-4
研究领域: 分析化学 · 材料科学
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CARBOHYDRATE POLYMERS · 2017 · IF 4.811

Controlled synthesis, immobilization and chiral recognition of carboxylic acid functionalized cellulose tris(3,5-dimethylphenylcarbamate)

Miaomiao Han,Xiaosa Jin,Han Yang,Xiao Liu,Yadong Liu,Shengxiang Ji

Traditional cellulose-based chiral stationary phases (CSPs) are prepared by physically coating cellulose derivatives onto substrates and only compatible with a very limited range of solvents as the mobile phase. Therefore, chemical immobilization of cellulose derivatives onto silica gel has been efficiently applied to improve the solvent compatibility of cellulose-based CSPs. Here we developed a novel approach to homogeneously modifying cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC). A series of carboxylic acid functionalized CDMPCs (CC-Xs) with controlled amounts and randomly distributed carboxylic acid groups was synthesized. CC-Xs were effectively immobilized onto amine-modified silica gel to afford immobilized CSPs. Compared to coated-type CSPs, immobilized CSPs significantly improved the solvent compatibility while maintaining similar chiral recognition abilities, but the introduction of excessive functional groups led to a deteriorated performance for columns. Moreover, a commercial drug, atenolol, was also sufficiently separated on the immobilized CSPs.

研究领域: 分析化学 · 有机化学
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JOURNAL OF CHROMATOGRAPHY A · 2018 · IF 3.716

A micro gas chromatographic column with embedded elliptic cylindrical posts

Bowen Tian,Bin Zhao,Fei Feng,Fan Luo,Haimei Zhou,Xiaohong Ge,Wu Yanhong,Xinxin Li

In this paper, a novel embeded elliptic cylindrical posts (ECPs) with large surface area and wide effective width, which could support more stationary phase and decrease the pressure drop, is applied on the micro-fabricated gas chromatographic (μGC) column. Compared with μGC column with cylindrical posts (CPs), the surface area and effective width of μGC column with ECPs are increased by 29% and 30%. Separation experiments are performed under the same head pressure at column inlet: in experiments of separating mixture 1, the column efficiency of the μGC column with ECPs for C9 has a 76% improvement, and the separation resolution between C8 and C9 also has a 34% improvement; in experiments of separating mixture 2, seven kinds of analytes can be identified by the μGC column with ECPs less than ten minutes, while, only six kinds can be identified by the μGC column with CPs in almost the same time. In detail, the column efficiency of the μGC column with ECPs for toluene has a 129% improvement, and the separation resolution between benzene and toluene also has a 56.4% improvement. Hence, the μGC column with the inner structures of ECPs is a valid means to improve column efficiency and resolution in a lower pressure drop.

CAS / MDL: 70131-67-8
研究领域: 分析化学 · 微流控技术
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

A micro gas chromatographic column with in-situ growing macro-porous silicon as stationary phase support layer

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

This paper reports a micro gas chromatographic column (μGCC) with in-situ growing macro-porous silicon as the stationary phase support layer. The macro-porous silicon stationary phase support layer (MPSL) with uniform thickness was fabricated in-situ on the inner surface of the μGCC channels by metal-assisted chemical etching. In order to avoid the negative effect of uneven thickness of the stationary phase, a 10 nm alumina film was deposited as the stationary phase on the MPSL using the atomic layer deposition technique. The macro-porous structure and high specific surface area of the MPSL provide longer diffusion paths and larger mass transfer interfaces for the analytes, which reduces the longitudinal gas diffusion and mass transfer resistance, thus improving the column efficiency. The μGCC with the MPSL achieved a 1306.7% increase in the theoretical plate number and a 195.0 % improvement in the resolution for n-nonane compared with the μGCC without the MPSL.

CAS / MDL: 75-15-0
研究领域: 分析化学 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2013 · IF 4.612

Tubular metal–organic framework-based capillary gas chromatography column for separation of alkanes and aromatic positional isomers

Zhi-Li Fang,Sheng-Run Zheng,Jing-Bo Tan,Song-Liang Cai,Jun Fan,Xia Yan,Wei-Guang Zhang

In this work, a tubular metal–organic framework, MOF-CJ3, with a large one-dimensional channel was chosen as stationary phase to prepare a capillary gas chromatographic column via a verified dynamic coating procedure. The column offered good separations of linear and branched alkanes, as well as aromatic positional isomers (ethylbenzene, xylene, cresol, hydroquinone, dichlorobenzene, bromobenzonitrile, chloronitrobenzene, and nitrotoluene) based on a combination of host–guest interactions and adsorption effects. Elution sequence of most of the analytes followed an increasing order of their boiling points, except for the separation of n -heptanes/isooctane, cresol, and hydroquinone isomers. Separation behavior of the column upon different organic substances may be related to the tubular pore structure of MOF-CJ3, in which the van der Waals forces between the alkanes and the hydrophobic inner surfaces might have great effect on separation of n -heptanes and isooctane, whereas the separation of cresol and hydroquinone isomers were affected by (OH⋯O) hydrogen bonds formed between the analytes and the 1,3,5-benzenetricarboxylate ligands on the pore wall. The effects of temperature on separation of aromatic positional isomers were investigated to elucidate entropy and enthalpy controlling of the separation process.

研究领域: 分析化学 · 材料科学
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