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Analytical Methods · 2016 ·Vol. 8 ·期 7 ·1572-1576 · IF 1.915

A colorimetric and ratiometric fluorescent probe for the rapid and sensitive detection of sulfite in sugar

Xiaoming Jiang,Junchao Xu,Youlai Zhang,Hongying Wang,Lintao Zeng,Yue Zhang

A colorimetric and ratiometric fluorescent probe was developed for the detection of sulfite in sugar. The probe underwent a Michael addition reaction with sulfite, which resulted in significant changes in fluorescence ratios. The probe displayed a fast response (within 30 s) and high selectivity towards sulfite over other anions and bio-thiols. The fluorescence intensity ratios were linearly related to the concentration of SO32− ranging from 0 to 15 μM, and the limit of detection was determined to be as low as 12 nM. The probe was employed to determine the concentration of sulfite in sugar with good recovery.

CAS / MDL: 105-56-6
研究领域: 分析化学 · 食品科学
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FOOD CHEMISTRY · 2016 · IF 4.052

Improvement of simultaneous determination of neutral monosaccharides and uronic acids by gas chromatography

Xin Wang,Lihui Zhang,Jingli Wu,Weiqi Xu,Xiaoqin Wang,Xin Lü

Although pre-column derivatization with n-propylamine and acetic anhydride combined with the gas chromatograph was a useful method for the analysis of monosaccharide composition, failure often occurs because of lack of detail information on the mechanism as well as the operating key point in derivatization process. In this study, the key points in the derivatization (lactonization time, the amount of n-propylamine and acetic anhydride) were investigated and optimized to improve the method. Under the optimal conditions, the derivatives of seven neutral monosaccharides and two uronic acids were simultaneouly obtained, after which they were well separated and detected by GC. It was also found that all derivatives of monosaccharides were stable even stored for 20   days. The linearity, sensitivity, precision, reproducibility and recovery rate of the improved method were evaluated. Thereafter, five polysaccharide samples from different sources were analyzed to validate the improved method.

CAS / MDL: 76-05-1 16940-66-2
研究领域: 分析化学 · 生物化学
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ANALYTICAL CHEMISTRY · 2022 · IF 8.008

Carboxyl-Based CPMP Tag for Ultrasensitive Analysis of Disaccharides by Negative Tandem Mass Spectrometry

Shanshan Ma,Fangya Chen,Meng Zhang,Hang Yuan,Gangfeng Ouyang,Wuduo Zhao,Shusheng Zhang,Yufen Zhao

Here, we develop a sensitive method for glucose-containing disaccharide analysis by 1-(4-carboxyphenyl)-3-methyl-5-pyrazolone (CPMP) derivatization using mass spectrometry. The intense anion of [M – H]− (m/z 759) was observed for CPMP-labeled disaccharides in a negative mode. After derivatization, its sensitivity was significantly increased with the limits of detection (LODs) and limits of quantification (LOQ) ranging from 3.90 to 8.67 ng L–1 and 12.99 to 28.92 ng L–1, respectively. During CID-MS/MS analysis, the fragment patterns of CPMP derivatized disaccharides in the negative mode were simpler and clearer than their counterparts in a positive mode, which further could be applied to distinct and relatively quantitative isomeric disaccharides with ultrahigh sensitivity and good reproducibility. The great linear relationships could be achieved under wider concentration ratios from 0.01 to 20 compared to the previous report. Eventually, the developed methodology was applicable to identify isomeric disaccharides in beers. No sucrose was discovered. All beers contain 1,4- and 1,6-linked disaccharides. Some of them also have a mixture of 1,2- and 1,3-linked disaccharides. Through the integration of statistical analysis, beers with different production processes were finally discriminated, and the relative quantification of isomaltose and maltose was realized. In general, this method is sensitive, fast, and reliable for the discrimination and relative quantification of isomeric disaccharides in complex matrices. This study provides a new idea for the structural analysis of oligosaccharides in food, plants, and animals and an important theoretical basis for the exploration of new functions of oligosaccharides.

CAS / MDL: 3371-50-4
研究领域: 分析化学 · 食品科学 · 分子生物学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2022 · IF 3.318

A LC-MS/MS method to simultaneously profile 14 free monosaccharides in biofluids

Hao Wang,Xi Zhang,Yingfei Peng,Baishen Pan,Beili Wang,David Haixiang Peng,Wei Guo

Monosaccharides are important players in cell metabolism and potential biomarkers. An effective tool to quantify monosaccharides is required in basic research and healthcare. In this study, we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay that could simultaneously quantify 14 free monosaccharides and evaluated its performance according to clinical guidance. The LC-MS/MS step separated and quantified 14 monosaccharides with 6 min. The coefficient of variation at the lower limit of quantification was less than 20% for each analyte. The R square values from linear regression analyses were all greater than 0.995. The validated assay was employed to profile free monosaccharides in conditioned media from cell culture and patient sera from glucose tolerance test. Both LO2 cells and HEK293 cells consumed D-glucosamine, D-glucose and produced D-glucuronic acid, N-acetyl-D-glucosamine. Additionally, LO2 cells produced D-mannose and L-fucose, whereas HEK293 cells consumed D-mannose. In patient sera from glucose tolerance test, the level of D-glucose increased significantly after glucose intake, but the levels of other monosaccharides didn’t. In conclusion, the LC-MS/MS assay we developed for 14-monosaccharide profiling met clinical requirements. The monosaccharide profiling results showed the distinct monosaccharide metabolism between liver and kidney cells, and the ignorable diet effect on 6 serum monosaccharides.

研究领域: 分析化学 · 代谢组学 · 临床医学
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MOLECULES · 2024 ·Vol. 29 ·期 10 ·2287 · IF 4.2

A Rapid and Accurate UHPLC Method for Determination of Monosaccharides in Polysaccharides of Different Sources of Radix Astragali and Its Immune Activity Analysis

Yali Guo,Lijun Wang,Kaishuang Liu,Meifang Li,Yibao Jin,Lifei Gu,Xie-An Yu,Shuhong Wang,Ping Wang,Bing Wang,Tiejie Wang

With the escalating demand for Astragalus polysaccharides products developed from Radix Astragali (RA), the necessity for quality control of polysaccharides in RA has become increasingly urgent. In this study, a specific method for the simultaneous determination of seven monosaccharides in polysaccharides extracted from Radix Astragali (RA) has been developed and validated using ultra-performance liquid chromatography equipped with an ultraviolet detector (UHPLC-UV) for the first time. The 1-phenyl-3-methyl-5-pyrazolone (PMP) derivatizations were separated on a C18 column (Waters ACQUITYTM, Milfor, MA, USA, 1.8 µm, 2.1 × 100 mm) using gradient elution with a binary system of 5 mm ammonium formate (0.1% formic acid)-acetonitrile for 24 min. Additionally, seven monosaccharides showed good linear relationships (R2, 0.9971–0.9995), adequate precision (RSD < 4.21%), and high recoveries (RSD < 4.70%). The established method was used to analyze 109 batches of RA. Results showed that the Astragalus polysaccharides (APSs) mainly consist of mannose (Man), rhamnose (Rha), glucose (Glu), galactose (Gal), arabinose (Ara), xylose (Xyl); and fucose (Fuc); however, their composition was different among RA samples from different growth patterns, species, growth years, and origins, and the growth mode of RA and the age of wild-simulated RA can be accurately distinguished by principal component analysis (PCA). In addition, the immunological activity of APSs were also evaluated jointly by measurement of the NO release with RAW264.7, with the results showing that APSs have a promoting effect on the release of NO and exhibit a significant correlation with Man, Glu, Xyl, and Fuc contents. Accordingly, the new established monosaccharides analytical method and APS-immune activity determination in this study can provide a reference for quality evaluation and the establishment of quality standards for RA.

CAS / MDL: 89-25-8
研究领域: 中药学 · 分析化学 · 免疫学
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CARBOHYDRATE RESEARCH · 2024 · IF 2.4

Sensitive, precise fingerprint profiling for monosaccharide analysis of Bacillus Calmette-Guérin polysaccharide and nucleic acid isolates

Lan Luo,Lisha Lin,Sheng Huang,Yunxi Zhou,Shengmei Yang,Yan Zhu,Lanyan Zhang,Donghua Xiong,Yongsheng Wu,Mingyi Wu

A sensitive and precise HPLC-DAD method with pre-column PMP derivatization was established and validated, for analyzing the polysaccharides in Bacillus Calmette-Guérin polysaccharide and nucleic acid (BCG-PSN) isolates, after acid hydrolysis. And the HPLC fingerprint profiling was used to analyze its monosaccharide composition. The monosaccharide concentration-peak area calibration curve was of good linearity (R 2  > 0.99), over the range of 0.016–0.08 mg/mL for mannose or 0.24–1.20 mg/mL for glucose, with high recovery of 93–105 % for quality control samples. The intra-day RSD values of mannose and glucose concentration were less than 2.5 % and 2.1 %, respectively, and their inter-day RSD values were less than 4.3 % and 2.2 %, respectively, and remained stable for up to 14 days. This method also remained durable against changes in chromatographic parameters, but it's susceptible to the flow rate of mobile phase. Additionally, the method was applied to analyze the content of mannose and glucose in 22 batches BCG-PSN powder and 17 batches BCG-PSN injection. The results showed that the HPLC-DAD fingerprint spectra of all the BCG-PSN powder and BCG-PSN injection samples had a high degree of similarity, with the similar indexes up to 0.999 and 0.998, respectively. The HPLC-DAD method with pre-column PMP derivatization is highly rapid, effective, visual, and accurate for determination of monosaccharide contents. The validated method was successfully applied to the analysis of polysaccharide in both BCG-PSN powder and injection.

CAS / MDL: 89-25-8
研究领域: 生物化学 · 药物分析 · 医学
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FOOD CHEMISTRY · 2022 · IF 9.231

Characterization of degradation products of carrageenan by LC-QTOF/MS with a hypothetical database

Na Yan,Xia Li,Chundi Zhou,Qin Jiang,Jiyu Li,Zhenqing Zhang,Yilan Ouyang,Duxin Li,Jianxiang Li

Carrageenan (CGN) belongs to the sulfated polysaccharides family that is commonly used in the food industry. For oligosaccharide analysis, a liquid chromatography quadrupole time-of-flight/mass spectrometry strategy was developed using a hypothetical database. There are 2100 structures in the developed hypothetical κ-CGN database. To eliminate false-positive results, three approaches were used, including size exclusion chromatography with mass spectrometry, which differentiates the loss of sulfated groups caused by the hydrolysis process or the ionization process. Profiling of acidic hydrolysis products of κ-CGN was found that after 12 h of HCl cultivation, the κ-CGN was hydrolyzed to oligosaccharides lower than the degree of polymerization 10, breaking the α-1,3-glycoside linkage and producing even-numbered oligosaccharides. Another finding was that the pH at which acidic hydrolysis is terminated affects the generation of even and odd oligosaccharides. Peeling reaction occurs at the reduction end 4-linked-3,6-anhydrous- d -galactose when adjusted to alkaline conditions, thus generating odd oligosaccharides.

CAS / MDL: 631-61-8
研究领域: 食品科学 · 分析化学 · 质谱分析
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2025 · IF 6.2

A Glucose Oxidase-Nanozyme Cascade System with Adjustable Interenzyme Spacing for Glucose Analysis

Xiao-Yu Han,Liu Zhang,Jie Yu,Wen-Jing Sun,Mei-Jing Chang,Gao-Ying Zhi,Dong-Hao Zhang

Here, glucose oxidase (GOD) is connected to Fe3O4 nanozyme by using epoxy cross-linkers as a spacer arm to construct a GOD-nanozyme artificial enzyme cascade system that is easy to separate magnetically. The dual-enzyme system can regulate the distance between GOD and nanozyme by changing the chain length of the cross-linker. The optimal interenzyme spacing of 2 nm has led to a significant increase in the cascade activity of the dual-enzyme system to 1400 U/mg, which is 2.5 times higher than the cascade activity of the free two enzymes. The GOD-nanozyme cascade system is applied to glucose assay, which has high sensitivity and selectivity for glucose with the lowest detection limit of 0.1 mM. Even in a system where the concentration of interfering substances is 10 times higher than that of glucose, the GOD-nanozyme cascade system can still specifically recognize glucose. The dual-enzyme system is used to establish a visual analysis device for glucose detection. The design of this visual analysis device provides a new strategy for the visual detection of glucose, which is of great significance for promoting the development of bioenzyme-nanozyme cascade systems in bioanalysis.

研究领域: 生物分析 · 纳米技术 · 酶学 · 生物传感器 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

A methylation-assisted gas chromatography-mass spectrometry strategy for comprehensive monosaccharide profiling in Polygonatum polysaccharides: Overcoming limitations of conventional chromatographic techniques

Liang Xu,Jinjian Yao,Zhen Wang,Songzi Xie,Jinmei Ou,Bin Wang

Conventional methods for analyzing monosaccharides, such as 1-Phenyl-3-methyl-5-pyrazolone (PMP) derivatization coupled with high-performance liquid chromatography (HPLC), struggle to detect ketoses and acidic sugars. This limitation hinders the precise structural analysis of polysaccharides in traditional Chinese medicine (TCM). A methylation-assisted Gas Chromatography-Mass Spectrometry (GC–MS) approach was developed to address this issue in the current study. By optimizing the methylation process and using GC–MS with a BR-17 column and an Electron Ionization (EI) source, simultaneous detection of ten different monosaccharides was achieved within 20 min. GC–MS profiling of monosaccharides generally gives two peaks per analyte, except in the cases of fructose and galacturonic acid. Notably, fructose (Fru) was identified for the first time in the polysaccharides of Polygonatum species: P. sibiricum at 18.55 μg/mg, P. cyrtonema at 16.90 μg/mg, and P. kingianum at 14.35 μg/mg, overcoming the limitations of the inability to detect ketoses in the PMP-HPLC method. Data analysis revealed distinct species-specific markers: P. kingianum polysaccharides (PKP) uniquely contained α -galacturonic acid (α-Gal: 19.95 μg/mg), whereas P. sibiricum polysaccharides (PSP) featured six monosaccharides, including glucose (Glc: 135.45 μg/mg), mannose (Man: 78.95 μg/mg), and ribose (Rib: 26.90 μg/mg), with a total of 299.50 μg/mg. P. cyrtonema polysaccharides (PCP) showed elevated levels of glucuronic acid (GlcA, 38.40 μg/mg). This derivatization-enhanced GC–MS method effectively fingerprints TCM polysaccharides, enabling clear differentiation of Polygonatum species through analysis of monosaccharide composition and total sugar content. This approach establishes clear structural distinctions, overcoming the limitations of conventional chromatographic techniques and enhancing the quality control and authentication of TCM polysaccharides.

CAS / MDL: 544-76-3
研究领域: 分析化学 · 碳水化合物化学 · 植物化学 · 中医药学 · 质谱分析
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Analysis & Sensing · 2023 · IF 0

Braiding Three-Dimensional Paper-Based Microfluidic Devices

Cuiyun Jia,Bin Li,Jie Pan,Fengjiao Zhu,Xue Bai,Xianming Liu,Bingcheng Lin,Yahong Chen,Yao Lu

Three-dimensional paper-based microfluidic devices have great potential in various applications, including point-of-care diagnostics, environmental monitoring, and tissue engineering. However, their fabrication is still limited to stacking and origami methods, in which auxiliary equipment is needed to maintain the layers in tightly connected junctions. Inspired by the art of bamboo braiding in China, we developed a novel fabrication technique based on the braiding concept to create three-dimensional paper-based microfluidic devices with PDMS-impregnated paper substrates as the building units. The resulting three-dimensional paper device brings unique advantages, including compactness, facile disassembly, and real-time flow visualization. The multiplexed glucose analysis with a braided device integrated with 16-switchable valves for flow control was further fabricated to demonstrate the device's applicability. We envision braiding-based fabrication technology opening new possibilities and bringing broad applications for three-dimensional paper microfluidic devices.

研究领域: 微流控技术 · 生物医学工程 · 分析化学 · 材料科学
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BIOSENSORS & BIOELECTRONICS · 2024 · IF 10.7

Synergistic Enhancement of Wearable Biosensor through Pt Single-Atom Catalyst for Sweat Analysis

Yong Zhang,Zhihao Yang,Cailin Qiao,Yiyi Liu,Cuncun Wang,Xin Zeng,Jingzhou Hou,Danqun Huo,Changjun Hou

Real-time monitoring of biological markers in sweat is a valuable tool for health assessment. In this study, we have developed an innovative wearable biosensor for precise analysis of glucose in sweat during physical activities. The sensor is based on a single-atom catalyst of platinum (Pt) uniformly dispersed on tricobalt tetroxide (Co 3 O 4 ) nanorods and reduced graphene oxide (rGO), featuring a unique three-dimensional nanostructure and excellent glucose electrocatalytic performance with a wide detection range of 1-800 μM. Additionally, density functional theory calculations have revealed the synergetic role of Pt active sites in the Pt single-atom catalyst (Co 3 O 4 /rGO/Pt) in glucose adsorption and electron transfer, thereby enhancing sensor performance. To enable application in wearable devices, we designed an S-shaped microfluidic chip and a point-of-care testing (POCT) device, both of which were validated for effectiveness through actual use by volunteers. This research provides valuable insights and innovative approaches for analyzing sweat glucose using wearable devices, contributing to the advancement of personalized healthcare.

研究领域: 生物传感器 · 催化 · 材料科学 · 纳米技术 · 健康监测 · 可穿戴技术
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Advanced Materials Interfaces · 2023 · IF 5.4

A Flexible and Wearable Chemiresistive Biosensor Fabricated by Laser Inducing for Real-Time Glucose Analysis of Sweat

HongXun Sun,Shujia Song,Guo Zhao,Xiaochan Wang,Gang Liu

In this study, a flexible and wearable chemiresistive biosensor (FWCB) is developed for the real-time analysis of glucose in sweat on the human skin surface based on a novel detection strategy of p -type reduced graphene oxide (rGO) sensing film, which met the requirements of rapid, nondestructive testing. The proposed FWCB is fabricated in the form of interdigital electrodes (IEs) made of laser-induced graphene (LIG) synthesized by the laser inducing of a polyimide (PI) film. Additionally, a semiconducting rGO sensing film modified on the surface of IEs is synthesized by thermal reduction of graphene oxide (GO), which is functionalized with glucose oxidase (GOx) by chemical cross-linking to obtain GOx/FWCB. Moreover, the key parameters for FWCB fabrication are optimized, and the sensing strategy of the proposed GOx/FWCB is also investigated. The results show that the proposed GOx/FWCB can be used for the detection of glucose in the range of 0.01–3.0 mM with satisfactory selectivity, and the limit of detection (LOD) is calculated to be as low as 0.8 µM (S/N = 3). These dramatic advantages endow the proposed FWCB with broad application prospects in the field of portable, wearable, and real-time detection of glucose in human sweat for health monitoring.

CAS / MDL: 141-43-5 98-79-3
研究领域: 生物传感器 · 材料科学 · 纳米技术 · 健康监测 · 可穿戴技术 · 分析化学
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