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FOOD AND BIOPRODUCTS PROCESSING · 2024 · IF 3.5

Efficient preparation of sophorose from fermentation broth via a newly developed integrated separation process

Lu Ren,Yang Hu,Yefei Wu,Mengqian Zhao,Qianqian Ma,Yulu Du,Jianwei Lu,Xuwei Long

Sophorose is a rare and valuable disaccharide with an unusual β -1,2 bond. Despite the relatively widespread interest in sophorose, the information regarding sophorose is limited because sophorose is not readily accessible. Thus, we used Candida bombicola ATCC 22214 for the efficient fermentative production of sophorose using glucose and soybean oil as substrates. In addition, an integrated separation process comprising precipitation, extraction, electrodialysis, and column chromatography was developed to purify the sophorose. Sophorose (approximately 35   g/L) was produced under optimized fermentation conditions in terms of the feeding strategy and enhanced mass-transfer efficiency. Thereafter, approximately 38% of sophorose (purity above 99%) was recovered from fermentation broth through the proposed process. This study provides an efficient approach for the large-scale preparation of sophorose, which is helpful for its practical application and in-depth research.

CAS / MDL: 8013-01-2
研究领域: 生物工程 · 糖化学
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INTEGRATED FERROELECTRICS · 2023 · IF 0.7

Modified Column Lamography Silicone Powder Separates Thiophene and its Derivatives

Xin-Yu Liu,Lin-Lin Kang,Hai-Lin Cong,You-Qing Shen,Bing Yu

Column laminating silica gel board plays a very important role in the separation and analysis of organic synthesis, which can monitor the progress of chemical reactions in real time and help researchers determine the time when chemical reactions are completed. In this work, we made a modified silicone powder for the separation and analysis of thiophene substances, and found that the modified silicone powder has a better separation effect than commercial silicone powder, which is expected to play a better role in the field of column chromatography separation.

研究领域: 化学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

A 3D-metal-printed UV detector specifically designed for real-time monitoring of an open column chromatography fraction

Yanting Liu,Xiaochun Li,Hongjun Luo,Rui Huang,Xuewan Wu,Lei Tan,Jialiang Guo,Kaisong Yuan

We developed a three-dimensional (3D)-metal-printed ultraviolet (UV) detector with an aluminum alloy housing that allows it to withstand low-polarity organic solvents. The detector can be attached to the lower end of an open chromatography column to realize real-time monitoring of the separated and eluted colorless fractions. Open column chromatography is commonly used for the separation and purification of mixtures. However, open column chromatography is never coupled with UV detectors. In the context of open chromatography column experiments, thin-layer chromatography (TLC) is typically employed for the qualitative analysis of separated products. Nevertheless, this approach is both cumbersome and time-consuming. Therefore, to reduce workload and save time, we developed a 3D-metal-printed UV detector, which exhibits good stability and linearity (R 2 > 0.99). The feasibility of real-time monitoring using this 3D-metal-printed UV detector was verified by subjecting the mixture to separation and monitoring. On elution of a substance exhibiting light-absorbing properties, a decrease in voltage is observed. At this point, the collection of the fractions may be initiated to achieve the effect of substance tracking. The utilization of the 3D-metal-printed UV detector for real-time monitoring enables the elimination of the time previously spent on the collection of all fractions and the subsequent determination of whether the fractions contain the substance by TLC. It is also capable of determining the separation effect of the mixture based on the curve monitored in real time. Moreover, the device can modify the dimensions of the interface, thereby facilitating its utilization in conjunction with high-performance liquid chromatography (HPLC) for the real-time monitoring of the separation effect of the column. The device is characterized by low cost and small size.

CAS / MDL: 103-90-2
研究领域: 分析化学 · 材料科学
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GREEN CHEMISTRY · 2023 ·Vol. 25 ·期 22 ·9363-9373 · IF 9.8

Scale-up preparation, column chromatography-free purification of protected carbonyl-containing biomass molecules and their derivatizations

Lei Huang,Chen Li,Zhidong An,Heqi Zhang,Dionisios G. Vlachos,Jiang Li

Recently, the protection strategy has received significant attention due to improved product selectivity and process efficiency for biomass conversion. In this work, an effective route to protect the carbonyl group of biomass-based furans with 1,3-propylene glycol followed by a simple but effective purification process is first established. Sulfamic acid, a commercially available, low-cost heterogeneous Brønsted acid catalyst, under different reaction conditions, exhibited excellent acetalization performance at gram level with good recyclability. Then, an efficient column chromatography-free purification protocol was established to give gram-level, high-purity acetal products by bypassing large eluent use, long processing times, and poor separation of strong polarity molecules by column chromatography. We further examined the protection group effect on selectivity during the hydrodeoxygenation, deoxygenation, or ring hydrogenation of biomass-derived furanic compounds over supports with different acidity/basicity under a reducing atmosphere that differs from previous reports that were typically focused on aerobic oxidation. Finally, the positive effect of the protection strategy on the photocatalytic oxidation of HMF is reported. Overall, our work greatly expands the application potential of the protection strategy via proposing an effective scale-up preparation method for commercially unavailable substrates and exploring more reaction types, especially under a reducing atmosphere. A grander blueprint to explore the protection strategy in biomass conversion can be imagined.

研究领域: 生物化学 · 绿色化学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2025 · IF 9

Development of a green and optimized process for isolating high-purity naringin and neohesperidin from Qu aurantii fructus

Ziwei Wang,Xiaojing Hou,Junxuan Jin,Yuchen He,Kejun Wu

This study introduces a green, optimized process for efficiently extracting high-purity naringin and neohesperidin from Qu Aurantii Fructus, a valuable traditional Chinese medicine. The total flavonoids from Qu Aurantii Fructus were extracted using ultrasonic-assisted ethanol extraction and subsequently purified with AB-8 resin, followed by the separation of high-purity naringin and neohesperidin through polyamide column chromatography. The investigation into the effect of ultrasound duration on the yield of total flavonoids revealed that at an ultrasonic duration of 25 min, the extraction yield of total flavonoids can reach its maximum. A thin-layer chromatography (TLC) system was employed to optimize the solvent system for the separation of naringin and neohesperidin, utilizing machine vision to assist in calculating and predicting the optimal solvent ratio, thereby simplifying the process and reducing variability and bias. The optimal solvent ratio (ethanol/ethyl acetate = 0.2848) was identified, leading to the successful isolation of high-purity naringin and neohesperidin (95.15 % and 99 %, respectively) through polyamide column chromatography and recrystallization. This process is devoid of toxic organic reagents, which enhances process safety and presents potential prospects for industrial applications, offering an efficient and eco-friendly method for the extraction and purification of valuable natural products

CAS / MDL: 7664-38-2
研究领域: 中药化学 · 天然产物分离纯化
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PROCESS BIOCHEMISTRY · 2024 · IF 3.7

Real-time monitoring of the column chromatography process of Ginkgo biloba using near-infrared and Raman spectroscopy combined with spectral fusion strategy

Sijie Zhang,Sheng Zhang,Xingchu Gong,Haibin Qu

In the column chromatography elution process of traditional Chinese medicine (TCM), the real-time monitoring of active components plays an important role in product quality control . In this study, the column chromatography elution process in preparing of Ginkgo biloba leaf extract was performed in bench scale, where near-infrared (NIR) spectroscopy and Raman spectroscopy were collected to determine the concentration changes of several critical quality attributes. Based on single spectral data and fused spectral data, partial least squares and support vector machine models were established, respectively. The results indicated that for most analytes, models based on Raman spectra were superior to NIR spectral models, and fusion models established by the mid-level data fusion approach were superior to the single spectral models. The coefficients of determination ( R t 2 ) of the optimal Raman and mid-level data fusion models were all higher than 0.96. The concentration profiles predicted by the mid-level data fusion quantitative models were in better agreement with the real trends defined by measured values. This is the first-ever study reporting the real-time monitoring of TCM column chromatography process by Raman spectroscopy combined with NIR spectroscopy, having vital reference values for process monitoring and understanding of the column chromatography for other TCM.

CAS / MDL: 7664-38-2
研究领域: 中药学 · 分析化学 · 光谱学
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MOLECULES · 2018 ·Vol. 23 ·期 5 ·996 · IF 3.098

Scale-Up Synthesis and Identification of GLYX-13, a NMDAR Glycine-Site Partial Agonist for the Treatment of Major Depressive Disorder

Wenchao Li,Jingjian Liu,Minghua Fan,Zhongtang Li,Yin Chen,Guisen Zhang,Zhuo Huang,Liangren Zhang

GLYX-13, a NMDAR glycine-site partial agonist, was discovered as a promising antidepressant with rapidly acting effects but no ketamine-like side effects. However, the reported synthetic process route had deficiencies of low yield and the use of unfriendly reagents. Here, we report a scaled-up synthesis of GLYX-13 with an overall yield of 30% on the hectogram scale with a column chromatography-free strategy, where the coupling and deprotection reaction conditions were systematically optimized. Meanwhile, the absolute configuration of precursor compound of GLYX-13 was identified by X-ray single crystal diffraction. Finally, the activity of GLYX-13 was verified in the cortical neurons of mice through whole-cell voltage-clamp technique.Keywords:GLYX-13;NMDA receptor;chromatography-free synthesis;crystal structure;whole-cell voltage-clamp

研究领域: 药理学 · 合成化学 · 神经科学
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TheScientificWorldJOURNAL · 2014 ·Vol. 2014 ·期 1 ·857982 · IF 1.219

Antioxidative Activities and Active Compounds of Extracts from Catalpa Plant Leaves

Hongyu Xu,Gege Hu,Juane Dong,Qin Wei,Hongbo Shao,Ming Lei

In order to screen the Catalpa plant with high antioxidant activity and confirm the corresponding active fractions from Catalpa ovata G. Don, C. fargesii Bur., and C. bungei C. A. Mey., total flavonoid contents and antioxidant activities of the extracts/fractions of Catalpa plant leaves were determined. The determined total flavonoid content and antioxidant activity were used as assessment criteria. Those compounds with antioxidant activity were isolated with silica gel column chromatography and ODS column chromatography. Our results showed that the total flavonoid content in C. bungei C. A. Mey. (30.07 mg/g·DW) was the highest, followed by those in C. fargesii Bur. (25.55 mg/g·DW) and C. ovata G. Don (24.96 mg/g·DW). According to the determination results of total flavonoid content and antioxidant activity in 3 clones of leaves of C. bungei C. A. Mey., the total flavonoid content and antioxidant activity in crude extracts from C. bungei C. A. Mey. 6 (CA6) leaves were the highest. Moreover, the results showed that the total flavonoid content and antioxidant activities of ethyl acetate (EA) fraction in ethanol crude extracts in CA6 leaves were the highest, followed by n -butanol, petroleum ether (PE), and water fractions. Two flavonoid compounds with antioxidant activity were firstly isolated based on EA fraction. The two compounds were luteolin ( 1 ) and apigenin ( 2 ), respectively.

研究领域: 植物化学 · 天然产物化学 · 药用植物学 · 抗氧化研究 · 分子生物学
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Foods · 2025 ·Vol. 14 ·期 23 ·4126 · IF 5.1

Structural Characterization and Immunomodulatory Activity of a Novel Mannoglucogalactan from Tremella aurantialba: Implications for Natural Immunotherapy

Yuemou Zhao,Wenyu Liang,Huaqun Chen,Jinwen Huang,Longyan Zhao,Qingxia Yuan

Heteropolysaccharides, the principal bioactive constituents of the esteemed medicinal foodTremella aurantialba, remain poorly understood in both structure and function. Herein, we describe a novel heteropolysaccharide, designated TAP-2a, isolated from the fruiting bodies ofT. aurantialbavia multi-step column chromatography. With a molecular weight of 16.95 kDa, TAP-2a is dominated by the pyranose forms of ᴅ-galactose (ᴅ-Galp), ᴅ-glucose (ᴅ-Glcp) and ᴅ-mannose (ᴅ-Manp), accompanied by minor proportions of ᴅ-xylose (ᴅ-Xylp), ʟ-fucose (ʟ-Fucp) and glucuronic acid. Methylation-GC-MS and exhaustive 1D/2D NMR analyses revealed a backbone assembled from →6)-α-Galp-(1→, →6)-β-Glcp-(1→, and →3)-α-Manp-(1→residues, branched at →2,6)-β-Galp-(1→, →3,6)-α-Galp-(1→, and →2,3)-α-Manp-(1→residues, and terminated by β-Glcp-(1→, α-Fucp-(1→, and β-Xylp-(1→. This intricate glycosidic architecture generates an exceptionally complex mannoglucogalactan in which a Gal→Man domain is substituted atO-3 of Gal by t-β-Glcpside chains and atO-2 of Man by t-α-Fucpstubs; additionally, a discrete fragment comprising t-β-Glcp-(1→3)-β-Glcp-(1→ was identified, along with a minor branch in which t-β-Xylpis attached toO-2 of a mannose residue. Functionally, TAP-2a proved to be a potent immunomodulator, markedly enhancing the secretion of nitric oxide, interleukin-1β, interleukin-6 and tumour necrosis factor-α while concurrently up-regulating the corresponding mRNA transcripts and augmenting phagocytic capacity. These findings establish the highly elaborate heteropolysaccharides ofT. aurantialbaas powerful immunomodulators that underpin the fungus’s renowned medicinal efficacy.

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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2017 · IF 2.603

Purification of quercetin-3-O-sophoroside and isoquercitrin from Poacynum hendersonii leaves using macroporous resins followed by Sephadex LH-20 column chromatography

Hongjuan Li,Ying Liu,Yuetao Yi,Qin miao,Sujing Liu,Feng Zhao,Wei Cong,Chunhua Wang,Chuanhai Xia

In China, Poacynum hendersonii is frequently used as a substitute for Apoacynum venetum L (Luobuma), which is a famous traditional Chinese medicine. Quercetin-3- O -sophoroside and isoquercitrin are two major flavonoids in Poacynum hendersonii leaves. In this work, a suitable method was established for the large-scale preparation of quercetin-3- O -sophoroside (QOS) and isoquercitrin (ISO) from Poacynum hendersonii leaves using macroporous resin combined with Sephadex LH-20 column chromatography. The adsorption/desorption capacities and desorption ratios of six macroporous resins were evaluated using static experiments. The HPD-300 resin had the best adsorption performance because it had the largest surface area, and was selected for further study. Compared with pseudo-first-order and intraparticle diffusion kinetics models, the pseudo-second-order model could better fit the adsorption kinetics of both QOS and ISO on the HPD-300 resin. In addition, the adsorption isotherms of the two compounds on the HPD-300 resin were fitted well to the Langmuir model. Under optimal conditions, the purities of QOS and ISO in the product were increased from 2.16% and 1.26% to 21.34% and 10.70% with recovery yields of 82.1% and 77.3%, respectively. Subsequently, Sephadex LH-20 column chromatography was employed for improving the purities of the two compounds. After separation by Sephadex LH-20 column chromatography, the purities of QOS and ISO achieved 93.5% and 95.6%, respectively.

研究领域: 药学 · 化学工程 · 天然产物化学 · 中药学
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JOURNAL OF SEPARATION SCIENCE · 2024 ·Vol. 47 ·期 3 ·2300741 · IF 2.8

Efficient discovery of active isolates from Dioscorea spongiosa by the combination of bioassay-guided macroporous resin column chromatography and high-speed counter-current chromatography

Zhenqiang Wang,Jinqian Yu,Lei Zhao,Tong Niu,Xiao Wang

In the present study, twelve compounds from Dioscorea spongiosa were successfully purified by an efficient technique combined bioassay-guided fractionation macroporous resin column chromatography (MRCC) pretreatment and high-speed counter-current chromatography (HSCCC) separation for the first time. Then, D101 MRCC was used to fractionate the crude extract into five parts, which further applied the bioassay-guided fractionation strategy to screen the active fractions of 2 and 4. As for the separation, 200 mg Fr.2 was purified by HSCCC using EtOAc/ n -BuOH/H 2 O (2:2:3, v/v), leading to annulatomarin ( 1 ), dioscoresides C ( 2 ), diosniponol C ( 3 ), methyl protodioscin ( 4 ), pseudoprotodioscin ( 5 ), protogracillin ( 6 ), as well as 200 mg Fr.4 yielding montroumarin ( 7 ), dioscorone A ( 8 ), diosniponol D ( 9 ), protodioscin ( 10 ), gracillin ( 11 ), and dioscin ( 12 ) using CH 2 Cl 2 /MeOH/H 2 O (3:3:2, v/v) with the purities over 95.0%. Finally, the isolates were assayed for their anti-inflammatory, urico-lowering, and anti-diabetic activities in vitro, which indicated that the steroidal saponins of 5 , 6 , and 11 showed all these three activities.

CAS / MDL: 7778-77-0 22767-49-3
研究领域: 生药学 · 天然产物化学 · 药理学
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES · 2023 · IF 8.2

Purification, structure identification and immune activity of a neutral polysaccharide from Cynanchum Auriculatum

Yilin Wang,Jin Han,Yun Yue,Yuze Wu,Wenqing Zhang,Wei Xia,Mengqi Wu

The crude polysaccharides CAPS and CAP of Cynanchum Auriculatum , which were prepared by degrading starch by single-enzymatic method (α-amylase) and double-enzymatic method (α-amylase and glucoamylase) respectively, were compared. CAP had good water solubility and higher non-starch polysaccharide content. A homogeneous neutral polysaccharide CAP-W, with the degree of acetylation about 17 %, was obtained from CAP by anion exchange column chromatography. Its detailed structure was identified by various methods. CAP-W, with the weight average molecular weight of 8.4 kDa, was composed of mannose, glucose, galactose, xylose, and arabinose in a molar ratio of 1.27:1.00:0.25:0.10:1.16. The backbone included β -1,4-Man p , β -1,4,6-Man p , β -1,4-Glc p and β -1,4,6-Glc p residues, with branches at the O-6 position of β -1,4,6-Man p and β -1,4,6-Glc p residues, consisting of α -T-Ara f , α -1,5-Ara f , α -1,2,5-Ara f , α -1,3,5-Ara f , T-Xyl p ,1,4-Xyl p , β -T-Man p and β -T-Gal p residues. In vitro immunological experiments suggested that CAP-W improved the phagocytic ability of macrophages, stimulated the release of NO, TNF-α and IL-6 from RAW264.7 cells, promoted the expression of NF-κB and caused nuclear translocation of NF-κB p65.

研究领域: 生物化学 · 免疫学 · 药理学 · 植物科学
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