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ANALYTICA CHIMICA ACTA · 2013 · IF 4.387

On-line coupling of macroporous resin column chromatography with direct analysis in real time mass spectrometry utilizing a surface flowing mode sample holder

Shanshan Zeng,Lu Wang,Teng Chen,Haibin Qu

A surface flowing mode sample holder was designed as an alternative sampling strategy for direct analysis in real time mass spectrometry (DART-MS). With the sample holder, the on-line coupling of macroporous resin column chromatography with DART-MS was explored and the new system was employed to monitor the column chromatography elution process of Panax notoginseng . The effluent from macroporous resin column was first diluted and mixed with a derivatization reagent on-line, and the mixture was then directly transferred into the ionization region of DART-MS by the sample holder. Notoginsenosides were methylated and ionized in a metastable helium gas stream , and was introduced into MS for detection. The on-line system showed reasonable repeatability with a relative standard deviation of 12.3% for the peak area. Three notoginsenosides, i.e. notoginsenoside R 1 , ginsenoside Rb 1 and ginsenoside Rg 1 , were simultaneously determined during the eluting process. The alteration of the chemical composition in the effluent was accurately identified in 9   min, agreeing well with the off-line analysis. The presented technique is more convenient compared to the traditional UPLC method. These results suggest that the surface flowing mode DART-MS has a good potential for the on-line process monitoring in the pharmaceutical industry .

CAS / MDL: 75-59-2
研究领域: 分析化学 · 中药学
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 43 ·期 4 ·839-846 · IF 2.516

Insight into molecular characteristics of a Chinese coal via separation, characterization, and data processing

Guo Yu,Xing Fan,Xue-Ming Dong,Rui-Yu Wang,Yun-Peng Zhao,Hong-Cun Bai,Tian-Sheng Zhao,Qing-Jie Guo,Xian-Yong Wei

Dayan lignite was subjected to thermal dissolution sequentially with cyclohexane, acetone, and methanol. Each thermal dissolution extract was subjected to further separation/enrichment using column chromatography, which was sequentially eluted with petroleum ether, a mixture of ethyl acetate and petroleum ether (vol:vol = 1:1), and ethyl acetate. The three thermal dissolution extracts and nine enrichment subfractions were characterized by an Orbitrap mass spectrometry equipped with an atmospheric pressure chemical ionization ion source. The mass spectrometry data were also statistically analyzed by principal component analysis, which can reduce the dimensionality of data and classify multiple samples according to principal components. Identified compounds in the extracts and subfractions are classified into eight classes according to the heteroatom distribution. Hydrocarbon class is mainly presented in the petroleum ether fraction, and oxygen class, nitrogen class, and oxygen-nitrogen class are distributed in both petroleum ether/ethyl acetate and ethyl acetate subfractions. The combination of different analytical methods enhances the understanding of coal at the molecular level and provides important data for downstream refining processes.

研究领域: 化学 · 能源科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2017 · IF 3.359

Separation of aromatic monomers from oxidatively depolymerized products of lignin by combining Sephadex and silica gel column chromatography

Ying Zhao,Xinping Ouyang,Jing Chen,Lisha Zhao,Xueqing Qiu

The conversion of lignin into value-added aromatic monomers has attracted much attention as these monomers can be potentially used to prepare liquid fuel rather than heavy oil by further hydrodeoxygenation. A new process combining Sephadex and silica gel column chromatography was employed to obtain aromatic monomers with higher purity. It was found that pH and polarity of mobile phase were the most important factors affecting the separation effect for Sephadex G-10 and silica gel column chromatography, respectively. When the pH of mobile phase reached 10.5, the ionization of hydroxyl together with carboxyl groups resulted in electrostatic repulsion between the aromatic compounds and Sephadex G-10 gel, which counteracted the adsorption caused by hydrogen bond between aromatics and gel, causing the increase of the separation effect. Under the condition of pH above 10.5, Sephadex gel column chromatography gave 78.1% of purity of aromatic monomers (PAM) and 99.5% of recovery of aromatic monomers (RAM) due to the elimination of non-size exclusion effect. Silica gel column chromatography was further conducted to obtain 99.8% of PAM and 73.9% of RAM. The polar mobile phase was favorable for eluting aromatic monomers, while the non-polar mobile phase was beneficial to remove oligomers and increasing the PAM.

研究领域: 生物化学 · 环境科学 · 材料科学
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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2023 ·Vol. 332 ·期 2 ·399-407 · IF 1.6

Selective adsorption of 99Tc and recovery of lanthanides at different acidity by PS-TMMA resin with double functional groups

Zu Jianhua,Pan Xiaohan,Han Gang,Xue Yi,Diao Jingjie,Liu Siyu

A novel resin (PS-TMMA) with double functional groups exhibited high adsorption selectivity toward 99 TcO 4 − from the coexisting fission products (Sr, Eu, Dy, Cs) in 0.1–1 mol/L HCl. On the contrary, in neutral medium K d of PS-TMMA resin towards lanthanide elements was much higher than Tc. The results of column chromatography showed that light lanthanide was firstly penetrated on the column. Using 0.01 mol/L 2-hydroxyisobutyric acid as eluent, the adsorbed lanthanides could be effectively eluted at pH 3.03, and the light and heavy lanthanides were partially separated in effluents.

研究领域: 放射化学 · 分离科学 · 核化学
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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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ACS Omega · 2022 · IF 4.132

Insights into a Low-Rank Naomaohu Coal Structural Information by Multistage Fractions Coupled with LIAD-VUVPI-TOFMS

Jingxiong Yu,Fanggang Liu,Zefeng Deng,Zaifa Shi,Jiangle Zhang,Qiaolin Wang,Jing Yang,Haoquan Hu,Zhengbo Qin,Zichao Tang

In-depth insights into the chemical composition and structural information of coal are an effective way to improve the efficiency of coal utilization. Laser-induced acoustic desorption coupling with vacuum ultraviolet photoionization time-of-flight mass spectrometry (LIAD-VUVPI-TOFMS) was applied to structural characterization of cyclohexane extracts of low-rank Naomaohu coal. The characterization of four types (12 model compounds) of mixed coal model compounds (three compounds per category)─saturated hydrocarbons, substitute aromatic hydrocarbons, aromatic hydrocarbons, and aromatic heteroatom rings─demonstrated that the approach can provide intact molecular weight information. The cyclohexanone extract (ECYC) was obtained by microwave-assisted extraction and separated into four group components (F1–4) by column chromatography to achieve component classification and simplify analysis. The molecular weight and structure were obtained by LIAD-VUVPI-TOFMS and synchronous fluorescence spectroscopy, combined with microwave-assisted extraction and column chromatography to separate product characteristics. Chemical components of a total of 248 species were observed, of which 46 are derived from aliphatic hydrocarbons embedded in the coal skeleton structure, 132 species are derived from aromatic hydrocarbons embedded in the coal skeleton structure, 61 are derived from possible coal skeleton units (compounds have obvious stacking and bonding effects), and 9 could not be determined (aromatic hydrocarbons or a possible coal skeleton structure unit).

研究领域: 燃料化学 · 分析化学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2024 ·Vol. 39 ·期 7 ·1938-1947 · IF 3.1

A two-step chromatographic purification method for Ni for its isotopic analysis by MC-ICP-MS

Lingke Li,Fei Wu,Yongsheng Liu,Tao He,Jie Lin,Wen Zhang,Rui Li,Haihong Chen,Keqing Zong,Zhen Zeng,Zhaochu Hu

Stable nickel (Ni) isotopes have shown great potential for investigating planetary accretion processes, mantle–crust magmatism, and paleo-marine evolution. The development of an economical and time-efficient separation method for Ni isotope analysis holds significant value within the realm of Ni isotope research. Previous purification methods for Ni isotope analysis have typically relied on either multi-column procedures or the utilization of significant quantities of organic reagents, such as acetic acid, acetone, and dimethylglyoxime. In this study, a novel two-column chromatographic separation procedure was presented for the determination of Ni isotope compositions in geological materials. A cation resin (AG50W-X8) was utilized in conjunction with diluted HCl and HF to effectively remove a substantial portion of matrix elements. Subsequently, trace amounts (100–200 μL) of Ni-spec resin were used for further purification of Ni. This relatively simple purification scheme for Ni isotope analysis effectively reduces the use of organic reagents and the amount of Ni-spec resin compared to previous methods that relied on multi-column separation and organic reagent extraction. Ni isotopic compositions were analyzed using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The instrumental mass discrimination of Ni isotopic ratios was corrected for using the double spike (DS) combined with the sample–standard bracketing (SSB) method. The Ni isotope compositions (δ60Ni) of in-house standards (SCP and CUG) were −0.06 ± 0.05‰ (2 SD, n = 104) and 0.36 ± 0.06‰ (2 SD, n = 97), respectively. Furthermore, the measured δ60Ni values of various geological reference materials (BCR-2, BHVO-2, BIR-1, DTS-1, DTS-2b, SDO-1, GSP-2, and W-2a from the USGS; JB-1b from the GSJ; GSR-2, GSR-3, GSR-4, GSR-5, and GSR-10 from the NRCGA) were consistent with previous studies within measurement error. Additionally, the δ60Ni values of AGV-1 from the USGS, as well as those of GSR-10, GSR-12, GSR-15, GSR-17, GSR-18, and GSR-19 from the NRCGA are reported here for the first time. Based on repeated measurements of pure solutions and reference materials, the long-term reproducibility of δ60Ni values was better than ± 0.06‰ (2 SD). Consequently, our study presents a relatively straightforward purification method for Ni for its isotopic analysis using only trace amounts of organic reagents and Ni-spec resin.

CAS / MDL: 34819-78-8
研究领域: 地球化学 · 同位素地球化学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2017 · IF 3.359

Chromatographic separation of glucose, xylose and arabinose from lignocellulosic hydrolysates using cation exchange resin

Kaifei Chen,Gang Luo,Zhongfang Lei,Zhenya Zhang,Shicheng Zhang,Jianmin Chen

Recovery of monosaccharides from hydrolysates of biomass wastes can bring environmental and economic benefits. This study aimed to explore the feasibility to separate major monosaccharides from hydrolysates of lignocellulosic biomass, i.e. glucose, xylose and arabinose by using column chromatography process. Cation exchange resin Amberlite IR120 and Amberlite IRP69 in Na + and Ca 2+ forms were chosen as adsorbents. The adsorption behaviors were firstly inspected by adsorption equilibrium and mass transfer coefficients. Then the optimal chromatography conditions were determined by using synthetic solution. Finally, hydrothermal liquefaction hydrolysate of pine branches was separated. The results showed that cation resin Amberlite IRP69 (Ca 2+ ) had high adsorption selectivity for arabinose which could be recovered from synthetic solution with purity of 92%. The highest purity of 88% was achieved for xylose when using this resin to separate pretreated hydrolysate. This work suggests that cation exchange resin could be further developed for effective separation of monosaccharides mixture.

研究领域: 生物化学 · 环境科学
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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Synthesis of polyethylene glycol functional bonded silica gel for selective recognition and separation of α-cyclodextrin

Xinying Zheng,Yang Qin,Xiaobing Meng,Zhengyu Jin,Liuping Fan,Jinpeng Wang

In this work, we for the first time synthesized the polyethylene glycol (PEG) bonded silica gel via KH-560 as a silane coupling reagent for column chromatography by a solid/liquid surface continuous reaction method. The molecular interaction, structure, morphology, and thermostability was characterized by fourier transform infrared spectroscopy (FTIR), elemental analysis (EA), scanning electronic microscope (SEM) and thermogravimetric analysis (TGA). Given that PEG is capable to self-assemble with α-CD, the PEG bonded silica gel was used as packing of column chromatography to achieve the selective separation of α-cyclodextrin (α-CD) at room temperature and atmospheric pressure. The bonded silica gel column could realize the effective separation of α-CD in the enzymatic hydrolysis mixture, which provides support for industrial separation of α-CD.

CAS / MDL: 10016-20-3 7646-69-7
研究领域: 化学 · 材料科学 · 分离技术
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SEPARATION SCIENCE AND TECHNOLOGY · 2021 · IF 2.475

Extraction and purification of pedunculoside from the dried barks of Ilex rotunda using crystallization combined with polyamide column chromatography

Weiyue Wang,Zenghao Yan,Hongliang Yao,Peibo Li,Wei Peng,Weiwei Su,Yonggang Wang

An efficient and low-cost method was developed for the preparation of pedunculoside from the dried barks of Ilex rotunda using crystallization combined with polyamide column chromatography. The kinetics of ethanol extraction was first evaluated and then the extract was concentrated to remove ethanol. Pedunculoside was partially crystallized after ethanol removal and those left in solution were further separated by polyamide column chromatography. To optimize the operating parameters for chromatography, the static and dynamic adsorption/desorption experiments were conducted. The purity of pedunculoside in the product increased to 85.69%, with an overall yield of 66.71%. The extraction and purification method developed herein provides a reference standard and can be used as the starting material for further studies.

CAS / MDL: 64-19-7
研究领域: 植物化学 · 分离科学 · 天然产物化学
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ACS Omega · 2020 · IF 2.87

Microwave-Assisted Preparation of Activated Carbon Modified by Zinc Chloride as a Packing Material for Column Separation of Saccharides

Ziwei Liu,Xiaoshun Zhou,Fengshou Wu,Zhimei Liu

Activated carbon, an amorphous carbon material with a high specific surface area and void fraction, is widely used as an economical adsorbent in many fields. In this work, a kind of new activated carbon composite for saccharide column separation was prepared by zinc chloride impregnating and microwave heating. The structural characterizations validate the increase in porosity and the specific surface area of the activated carbon as well as the change of the activated carbon crystallite lattice. The chemical characterizations validate the increase in the number of oxygen-containing functional groups and structural bonding of zinc with the activated carbon surface. Compared with the blank control, the surface Zn element improves the adsorption selectivity of the activated carbon to the target saccharides. Under the special mechanism of microwaves, the pores created by expansion from the inside to the outside facilitate the free flow of the mobile phase. The eight saccharides can be separated by the columns packed with the activated carbon impregnated with 40% and 70% zinc chloride.

CAS / MDL: 7646-85-7
研究领域: 材料科学 · 分析化学
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PHYTOCHEMICAL ANALYSIS · 2024 ·Vol. 35 ·期 6 ·1428-1442 · IF 3

An effective and comprehensive optimization strategy for preparing Ginkgo biloba leaf extract enriched in shikimic acid by macroporous resin column chromatography

Sijie Zhang,Xingchu Gong,Haibin Qu

Introduction Previously reported preparation methods of Ginkgo biloba leaf extract (EGBL) have mainly focused on the enrichment of flavonoid glycosides (FG) and terpene trilactones (TT), which led to the underutilization of G. biloba leaves (GBL). Objectives To make full use of GBL, in this study, a comprehensive optimization strategy for preparing EGBL by macroporous resin column chromatography was proposed and applied to enrich FG, TT, and shikimic acid (SA) from GBL. Methodology Initially, the static adsorption and desorption were executed to select suitable resin. Then, the influences of solution pH were investigated by the static and dynamic adsorption. Subsequently, eight process parameters were systematically investigated via a definitive screening design (DSD). After verification experiments, scale-up enrichment was carried out, investigating the feasibility of the developed strategy for application on an industrial scale. Results It was found that XDA1 was the most appropriate adsorbent for the preparation of EGBL at solution pH 2.0. Furthermore, based on the constraints of the desired quality attributes, the optimized ranges of operating parameters were successfully acquired, and the verification experiments demonstrated the accuracy and reliability of using DSD to investigate the chromatography process for the preparation of EGBL. Finally, magnified experiments were successfully performed, obtaining the EGBL containing 26.54% FG, 8.96% TT, and 10.70% SA, which reached the SA level of EGB761, an international standard EGBL. Conclusion The present study not only provided an efficient and convenient approach for the preparation of EGBL enriched in SA but also accelerated efforts to high-value utilization of GBL.

CAS / MDL: 7664-38-2
研究领域: 植物化学 · 中药学 · 分离纯化技术
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