ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
·
2020
·
IF 4.872
Lijun Liu,Junhui Chen,Xiuping He,Shuang Hao,Ziru Lian,Baodong Wang
Paralytic shellfish poisoning (PSP) toxins have received considerable attention in recent years because of their adverse effects on marine breeding industries and human health. In this study, a reliable method for the analysis of extracellular PSP toxins in the culture medium of marine toxic dinoflagellates was developed for the first time using graphitized carbon black–solid-phase extraction and hydrophilic interaction liquid chromatography–high-resolution mass spectrometry. The limit of quantification of typical PSP toxins in algal culture medium ranged from 0.072 μg/L to 0.151 μg/L under optimal conditions. Satisfactory absolute recoveries (87.5%–102.4%), precision (relative standard deviation ≤ 7.6%), and linearity ( R 2 ≥ 0.9998) were also achieved. In addition, the proposed method was applied to screen and determine the extracellular PSP toxins of two typical toxigenic dinoflagellates, Alexandrium minutum and Alexandrium tamarense . The total concentrations of the extracellular PSP toxins in A. minutum and A. tamarense over the whole growth period were within 2.0–735.5 and 2.0–19.2 μg/L, respectively. The concentrations of extracellular PSP toxins varied remarkably in the different growth stages of A. minutum and A. tamarense , and the contents of some extracellular PSP toxins were substantially higher than those of intracellular PSP toxins. Therefore, the extracellular PSP toxins released by toxigenic red tide algae cannot be ignored, and their environmental fate , bioavailability , and potential harm to aquatic environment need to be investigated in future studies.
研究领域:
海洋生物学
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环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
CARBOHYDRATE POLYMERS
·
2024
·
IF 10.7
Xi-yang Tang,Zhi-heng Shu,Peng-cheng Zhao,Wen Wei,Cai-lian Fan,Zhi-hong Yao,Xin-sheng Yao,Yi Dai
Zhu-Ling decoction (ZLD), a classical traditional Chinese medicine (TCM) formula, is used for the treatment of chronic kidney diseases. However, the structure and activity of absorbed oligosaccharides (OSs) in ZLD are not clear. In this study, a novel strategy with in vivo characterization, extraction, isolation, activity evaluation was established and applied to identify absorbed anti-inflammatory OSs in ZLD. The results revealed that 30 OSs (22 reducing and 8 non-reducing OSs) and 11 OSs (7 reducing and 4 non-reducing OS) were characterized from ZLD in vitro and in vivo by using UPLC/Q-TOF-MS with PMP derivatization, respectively. Among them, a series of −1 → 3- β -D-Glcp-OSs were isolated and identified by HPLC-HILIC-UVD-ELSD, SPHPLC-HILIC-RID, monosaccharide composition, MS and 1D/2D-NMR spectroscopy, including laminaritriose, laminaritetraose, laminaripentaose, laminarihexaose, laminariheptaose, laminarioctaose and laminarinonaose. Moreover, the 4 non-reducing absorbed OSs were identified by comparison with reference standards, including sucrose, trehalose, raffinose and stachyose. Among them, laminaritriose, laminaritetraose and laminaripentaose significantly inhibited TNF-α and IL-6 levels in LPS-induced HK-2 cell and exerted significant anti-inflammatory effects via the NF-κB and Akt/mTOR signaling pathways. Together, our work provides a novel strategy for discovery of absorbed anti-inflammatory OSs and broadens new horizons for the discovery of in vivo pharmacodynamic substances in TCM formulas.
研究领域:
药理学
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中药学
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生物化学
·
分子生物学
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产品关联
DOI
PubMed
高影响因子
CARBOHYDRATE POLYMERS
·
2021
·
IF 9.381
Yuerong Yang,Yu Lu,Yinchuan Liu,Yu Pan,Hongjuan Ma,Linjuan Huang,Zhongfu Wang
Yak milk (YM) has higher protein content than other bovine milk (BM) varieties. The bioactivity of milk glycoproteins is related to N / O -glycans. We qualitatively and quantitatively compared the N / O -glycome of YM and BM glycoproteins using stable isotope labeling combined with hydrophilic interaction chromatography and electrospray ionization mass spectrometry. We identified 79 and 78 N -glycans in YM and BM, respectively. Two N -glycans (H4N5F1A1; H5N4F1) were exclusive to YM. The content ratios of different types of N -glycans differed significantly between YM and BM, with sialylated N -glycans 2.33 times more abundant in YM. Five and seven O -glycans were detected in YM and BM, respectively. Two O -glycans (H1N2; H1N2A1) were exclusive to BM. The bi-sialylated O -glycan, H1N1A2, accounted for 56.1% of O -glycans in YM; it was 5.97 times more abundant in YM than in BM (equal volume basis). This study provides a theoretical basis for the future utilization of YM as a functional food.
研究领域:
食品科学
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生物化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Chunmiao Bo,Xiaomeng Wang,Chaozhan Wang,Yinmao Wei
Development of mixed-mode chromatography (MMC) stationary phase with adjustable selectivity is beneficial to meet the needs of complex samples. In this work, surface-initiated atom transfer radical polymerization (SI-ATRP) using the mixture of two functional monomers was proposed as a new preparation strategy for MMC stationary phase with adjustable selectivity. The mixture of sodium 4-styrenesulfonate (NASS) and dimethylaminoethyl methacrylate (DMAEMA) underwent SI-ATRP to bond poly(NASS-co-DMAEMA) on the surface of silica to prepare hydrophilic interaction/ion-exchange mixed-mode stationary phase. Various analytes (neutral, acidic, basic analytes and strong polar nucleosides) were employed to investigate the retention behaviors. The influences of water content and pH of the mobile phase on the retention validated the mixed-mode retention mechanisms of HILIC and ion-exchange. The charge and polarity of stationary phase as well as the separation selectivity were conveniently manipulated by the ratio of NASS to DMAEMA monomer, and the use of DMAEMA in the mixture additionally endowed the column with the temperature-responsive characteristics. Moreover, the application of the developed column was demonstrated by the successful separation of nucleosides, β-agonists and safflower injection. In a word, the proposed strategy can be potentially applied in the controllable preparation of MMC stationary phase with adjustable selectivity.
研究领域:
分析化学
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材料科学
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产品关联
DOI
PubMed
高影响因子
Foods
·
2024
·Vol. 13
·期 5
·635
·
IF 4.7
Aiping Li,Chen Wang,Zhenghao Wu,Yingying Liu,Zhenxia Hao,Chengyin Lu,Hongping Chen
Ningnanmycin is a widely used antibiotic in agricultural production that effectively controls fungal and viral diseases in tea trees and chrysanthemums. The polarity characteristic of ningnanmycin has posed limitations on the development of robust detection methods, thereby hindering effective monitoring and control measures. By combining cation exchange solid phase extraction (SPE) with hydrophilic interaction chromatography tandem mass spectrometry (HILIC-MS/MS), we have effectively tackled the issue pertaining to the separation and retention of ningnanmycin. The average recoveries of ningnanmycin in green tea, black tea, and chrysanthemum were 77.3–82.0%, 80.1–81.5%, and 74.0–80.0%, respectively. The intraday and interday relative standard deviations (RSDs) were below and equal to 7.7%. Good linearity was observed in the concentration range of 1–1000 μg/L (R2 > 0.998). The limits of detection (LODs) ranged from 1.1 μg/kg to 7.1 μg/kg, and the limits of quantification (LOQs) ranged from 3.6 μg/kg to 23.7 μg/kg for ningnanmycin. These results indicate the good accuracy, repeatability, reproducibility, and sensitivity of the method. It is suitable for detecting ningnanmycin in tea and chrysanthemum.
研究领域:
分析化学
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食品科学
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植物保护
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Zhenyao Lu,Sijia Li,Nan Aa,Yuanmao Zhang,Ran Zhang,Chen Xu,Shize Zhang,Xiangqing Kong,Guangji Wang,Jiye Aa,Yue Zhang
Purine and pyrimidine metabolism are vital metabolic pathways in the development, proliferation or repairment of cells or tissues associated with various diseases. Here, a simple, all-in-one injection hydrophilic interaction liquid chromatography-tandem mass spectrometry method was developed for simultaneous determination of 20 metabolites: adenine , adenosine, deoxyadenosine , adenosine 5′-monophosphate, cyclic adenosine monophosphate, hypoxanthine , xanthine , inosine , deoxyinosine , xanthosine , xanthosine 5′-monophosphate and uric acid , which are products of purine metabolism; uridine , deoxyuridine , uridine 5′-monophosphate and uracil , are products of pyrimidine metabolism; and corticosterone , methionine , acetylcholine and serotonin. To minimize interference of endogenous molecules in sample matrixes, a combination of activated carbon adsorption and a serum substitute matrix (5% bovine serum albumin in phosphate buffered saline) was utilized and jointly applied. The sensitivity, linearity, stability, precision, accuracy and extraction recovery were evaluated, and the method was demonstrated to be accurate, sensitive and reliable. An analytical strategy was successfully applied to quantitatively determine 20 metabolite levels in the serum and hippocampus of mice with chronic social defeat stress-induced depression. The results showed greatly perturbed purine metabolism in the depressed mice, which was primarily characterized by dramatic increases in hypoxanthine, xanthine and inosine in serum and reduced levels of adenine, adenosine and adenosine 5′-monophosphate in the hippocampus. These findings suggest that this novel strategy can facilitate the quantitative analysis of adenine and other purine and pyrimidine metabolites in tissue and serum and exhibits great potential in the exploration of metabolism-related mechanisms of relevant diseases.
研究领域:
生物化学
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医学
·
神经科学
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DOI
高影响因子
TALANTA
·
2020
·
IF 5.339
Fangbin Fan,Licheng Wang,Yijing Li,Xusheng Wang,Xiaofeng Lu,Yong Guo
l -Cysteine (L-Cys) and N-Isopropyl acrylamide (NIPAM)-modified silica spheres as a novel stationary phase for hydrophilic interaction liquid chromatography (HILIC) was produced firstly by cross-linking polymerization. Some characterizations in this article confirmed that the synthesis of Cys-Si-NIPAM is successful. Some polymer layers can be observed through transmission electron microscopy (TEM). In addition, through nitrogen adsorption porosity method, scanning electron microscopy (SEM), thermal gravimetric analysis (TGA) and other characterization methods, we can find the significant changes after modify. It has good hydrophilic property and higher column effect than bare silica column, Si-Cys column and Si-NIPAM column under the same conditions. It has good separation effect for some hydrophilic analytes such as 5 nucleosides and nucleoside bases, 5 amino acids , 4 sulfonamide drugs and 10 saccharides . The effects including column temperature, pH and organic solvent content on chromatographic performance were studied, which proved that hydrophilic interactions can be simultaneously existed between the stationary phase and the analytes. In addition, reproducibility and efficiency of the Cys-Si-NIPAM column was also investigated, the results illustrated that the stationary phase have passable stability (the intraday RSDs 0.08–0.44%, n = 3 and the interday RSD 0.46–3.50%, n = 3) and ideal efficiency (plates per meter, ~45700 plates/m). In conclusion, the preparation process of this hydrophilic liquid chromatography stationary phase is not only simple, but also can meet the basic requirements for the separation of hydrophilic analytes.
研究领域:
分析化学
·
色谱技术
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Xiang Wang,Xingrui Wang,Hanqi Yang,Hanlin Zeng,Zhiqiang Xu,Wenhao Chen,Guangming Zhou,Jingdong Peng
In this study, we synthesized and employed an ionic gel-functionalized silica stationary phase for high-performance liquid chromatography. The successful fabrication of the stationary phase was confirmed through attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), zeta-potential measurements, and elemental analysis (EA). Comparative performance evaluation against a commercial column demonstrated the prepared column's effectiveness in the mixed mode of reversed-phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), and ion chromatography (IC). Moreover, the stationary phase exhibited exceptional retention repeatability in per aqueous liquid chromatography, showcasing its potential as an environmentally friendly analytical method. Mechanistic investigations unveiled multiple solute-stationary phase interactions, including π-π interactions, hydrogen bonding, and ion exchange. Finally, we applied the developed stationary phase for the precise detection of preservatives in carbonated beverages and jelly, achieving high levels of accuracy and recovery rates.
研究领域:
分析化学
·
环境科学
·
食品科学
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产品关联
DOI
PubMed
高影响因子
CARBOHYDRATE POLYMERS
·
2023
·
IF 11.2
Zhenhua Li,Xiaoqin Wang,Xiaoli Deng,Jiansen Song,Tong Yang,Yujie Liao,Guiping Gong,Linjuan Huang,Yu Lu,Zhongfu Wang
Glycosphingolipids (GSLs) in human milk regulate the immune system, support intestinal maturation, and prevent gut pathogens. The structural complexity and low abundance of GSLs limits their systematic analysis. Here, we coupled the use of monosialoganglioside 1–2-amino-N-(2-aminoethyl) benzamide (GM1-AEAB) derivatives as internal standards with HILIC-MS/MS to qualitatively and quantitatively compare GSLs in human, bovine, and goat milk. One neutral glycosphingolipid (GB) and 33 gangliosides were found in human milk, of which 22 were newly detected and three were fucosylated. Five GB and 26 gangliosides were identified in bovine milk , of which 21 were newly discovered. Four GB and 33 gangliosides were detected in goat milk, 23 of them newly reported. GM1 was the main GSL in human milk; whereas disialoganglioside 3 (GD3) and monosialogangloside 3 (GM3) were dominant in bovine and goat milk, respectively; N -acetylneuraminic acid (Neu5Ac) was detected in >88 % of GSLs in bovine and goat milk. N -hydroxyacetylneuraminic acid (Neu5Gc)-modified GSLs were 3.5 times more abundant in goat than in bovine milk; whereas GSLs modified with both Neu5Ac and Neu5Gc were 3 times more abundant in bovine than in goat milk. Given the health benefits of different GSLs, these results will facilitate the development of custom-designed human milk-based infant formula.
研究领域:
营养学
·
生物化学
·
代谢组学
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DOI
PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2020
·
IF 9.038
Fei Long,Mei Zhang,Jiahao Yuan,Juan Du,Ande Ma,Jialiang Pan
The measurement of trace hydrophilic toxins in complex aqueous-rich matrices is a daunting challenge. To address this analytical bottleneck, pulse diffusion focusing (PDF), a novel sample injection technique for hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/MS), was developed. Theoretical and experimental investigations of the mechanism and key parameters revealed that the pulse-injection approach, assisted by solvent diffusion, efficiently solved the volume overload problem. This milliliter-level-injection HILIC-MS/MS technique was reported for the first time herein, and provided a significant enhancement in sensitivity compared to the conventional injection method, in addition to being an efficient approach to address the solvent incompatibility of off-line sample preparation and HILIC . The automated PDF-HILIC-MS/MS system was obtained by slightly modifying a commercial LC–MS/MS instrument in an easy and economical manner. The efficiency of the system was demonstrated through the detection of trace tetrodotoxin contents in plasma and urine samples. Low limits of detection (i.e., 0.65 and 2.2 ng·mL −1 ) were obtained using the simplified sample preparation method. The recoveries were in the range 91–113.3 % with intra-day and inter-day precisions of ≤9.6 %. Further experimental results proved the method to be versatile for various hydrophilic toxins.
研究领域:
分析化学
·
毒理学
·
医学检测
✓ 已验证
DOI
高影响因子
CHROMATOGRAPHIA
·
2025
·
IF 1.3
Lou Doudou,Zhu Yuan,Fan Jingke,Fan Lin,Zhu Qingfu,Lu Yihong,Zhao Shuqiang
N-glycosylation heterogeneity has a significant impact on the clinical safety, efficacy, pharmacokinetics (PK), and pharmacodynamics of monoclonal antibody (mAb) drugs, thus becoming a critical quality attribute (CQA) of great concern. In the registration quality standards for bevacizumab produced by different manufacturers, either lacking supervision of N-glycosylation or the detection methods and criteria vary greatly among manufacturers, leading to compromised comparability of results. Besides, the existing quality control system pays insufficient attention to the correlation between glyco-relevant physicochemical properties and glycosylated modification. In this study, a standardized hydrophilic interaction liquid chromatography-fluorescence detection (HILIC-FLD) N-glycan profiling method was developed, which had been proven to be more time-saving and easier to operate and was used for the parallel analysis of N-glycan profiles in bevacizumab products provided by 8 different manufacturers. We also paid attention to the glycosylation-related CQAs including charge heterogeneity, isoelectric point, non-glycosylated heavy chain (NGHC) and aggregates. Results revealed obvious difference in N-glycosylation, NGHC and aggregates among manufacturers. Among all the mAbs, the abundance of major glycoforms showed similar order yet the percentage of the same glycoform varies greatly. In summary, the standardized method could offer a reliable, efficient and practical approach for the parallel analysis and comparison of glycosylation and related CQA heterogeneity among manufacturers, providing a reference for more effective quality control of mAb drugs.
研究领域:
生物化学
·
药物分析
·
分子生物学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Yilin Zhang,Mengqi Wu,Jingrui Xi,Chen Pan,Zhizhen Xu,Wei Xia,Wenqing Zhang
In this study, the multiple fingerprints, which were integrated with HPGFC-ELSD (high performance gel filtration chromatography - evaporative light scattering detector) fingerprint, PMP-HPLC-DAD (1-phenyl-3-methyl-5-pyrazolone-high performance liquid chromatography - diode array detector) fingerprint of complete acid hydrolysates and HILIC-HPLC-ELSD (hydrophilic interaction - high performance liquid chromatography - evaporative light scattering detector) fingerprint of enzyme hydrolysates, were established to evaluate the quality of polysaccharides from Poria cocos (PCPs). The similarity evaluation showed that 16 batches of PCPs from different origins had high similarity in structural characteristics based on the multiple fingerprints. The chromatographic data of multiple fingerprints of PCPs were fused, processed and analyzed by chemometric methods including HCA (hierarchical cluster analysis), PCA (principal component analysis) and PLS-DA (partial least squares discriminant analysis). The 16 batches of PCPs were divided into 3 categories in PCA, indicating a certain relationship between the structural characteristics and the origins. PLS-DA analysis indicated that Man, Glc, Gal, Fuc, the components with m/z of 2.22 × 10 4 ∼1.53 × 10 4 Da and 3.46 × 10 3 ∼2.69 × 10 3 Da, oligosaccharides with DPs of 6 and 7, respectively, could be regarded as potential chemical markers for the classification of PCPs from different origins. According to the multiple fingerprints and chemometric analysis, the two commercial samples were proved to be adulterants.
研究领域:
中药学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）