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ANALYTICA CHIMICA ACTA · 2022 · IF 6.911

Speciation of organotin compounds in water and seafood samples by online hyphenation of porous polymer-based magnetism-enhanced in-tube solid phase microextraction and HPLC

Xiaochong Song,Qing Luo,Xiaojia Huang

A new strategy based on online hyphenation of magnetism-enhanced in-tube solid phase microextraction (ME-SPME) and HPLC was developed for speciation of organotin compounds (OTCs) in water and seafood samples. Task specific porous polymer embedded magnetic nanoparticles (TPM) was fabricated in capillary and utilized as the microextraction column (MEC) of ME-SPME. The implement of magnetic field during extraction duration obviously improved extraction efficiencies of prepared TPM/MEC towards studied TOCs from 48.0-77.0% to 84.2–99.7%. Under the optimized extraction parameters, sensitive and automatic approach for the quantification of TOCs was developed by online hyphenation of ME-SPME and HPLC with fluorescence detection. The limits of detection for water and seafood samples were in the ranges of 0.0030–1.5 μg/L and 0.71–14 μg/kg, respectively. The established method was employed to measure low contents of studied OTCs in actual samples, and the recoveries at different fortified contents varied from 80.2% to 116% with satisfactory reproducibility (RSDs below 10%). In addition, confirmation experiments were adopted to inspect the accuracy of introduced method.

研究领域: 分析化学 · 环境科学 · 食品科学
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2025 · IF 3.2

Determination of seven fatty acids in plasma of rats after oral administration of Xanthoceras sorbifolia bunge oil by GC-MS and pharmacokinetic study

Guo Shuang,Qiao Xuan,Lv Zihan,Li Lintao,Liang Yutong,Meng Zhiyun,Gan Hui,Gu Ruolan,Wu Zhuona,Dou Guifang,Li Gaoying,Liu Shuchen

This work aims to establish a highly selective, sensitive, and accurate gas chromatography-mass spectrometry (GC-MS) method for detecting concentrations of seven representative fatty acids absorbed into the bloodstream after a single gavage of 10 mL/kg Xanthoceras sorbifolia Bunge ( X.sorbifolia ) oil in rats and conducting pharmacokinetic studies. The plasma samples were processed using two-step derivatization with NaOH and BF 3 -CH 3 OH, with an Agilent HP-88 capillary column serving as the stationary phase. Concentrations of seven fatty acids, namely hexadecanoic acid (palmitic acid, C16:0), octadecenoic acid (stearic acid, C18:0), cis -9-octadecenoic acid (oleic acid, C18:1), cis -9,12-octadecadienoic acid ( linoleic acid, C18:2), cis -11-eicosenoic acid (gondoic acid, C20:1), cis -13-docosaenoic acid (erucic acid, C22:1), and cis -15-tetracosenoic acid (nervonic acid, C24:1), were quantitatively determined under programmed temperature and ion detection mode. The results showed that the seven fatty acids were well separated and exhibited a good linear relationship between concentration and peak area ratio within the detection range (R 2  > 0.99). The precision and accuracy within and between batches were both less than 15%. After derivatization, the plasma samples remained stable at -20 °C, 4 °C, and 10 °C; The matrix effect did not affect the quantitative analysis, and the extraction recovery rate ranged from 100.3% to 107.76%. After gavage administration of X.sorbifolia oil to rats, the levels of unsaturated fatty acids in the blood were significantly increased compared to those in the blank control group. The peak concentration (T max) was 7–8 h, and the mean retention time (MRT) was 10–12 h. This experiment provides a basis for elucidating the potential material basis of the nutritional efficacy of X. sorbifolia oil after oral administration.

CAS / MDL: 112-63-0
研究领域: 分析化学 · 药理学 · 生物化学 · 营养学 · 药物化学
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JOURNAL OF CHROMATOGRAPHY A · 2022 · IF 4.601

Simultaneous quantification of plasma immunoglobulin subclasses for assessment of maternal and fetal immune response during pregnancy

Jialing Huang,Yunqing Qi,Xiaowen Zeng,Wei Huang,Da Chen

Measurement of immunoglobulin subclasses is a useful tool for exploring humoral immune deficiency in the presence of total immunoglobulins within reference intervals. Conventional methods for immunoglobulin measurement are mostly immunoassays, which are of low throughput and laborious to run multiple immunoglobulin subclass tests. Liquid chromatography-mass spectrometry (LC-MS) has emerged as a promising technology for the measurement of protein biomarkers in biological matrices, owing to its high specificity, selectivity, multiplexing, and wide dynamic range. In fully taking these advantages, we developed here a LC-MS based methodology for simultaneous quantitation of the primary immunoglobulin isotypes (IgG, IgA, IgM) and their subclasses in human plasma. Method validation demonstrated that the proposed method showed good linearity with R  > 0.99, high precision with coefficients of variation for inter- and intra-assay less than 15%, as well as high accuracy with relative errors less than 8.7%. The developed method was further applied to maternal and cord blood collected at delivery for assessment of maternal and fetal immune status. The immunoglobulin profiles and the features of transplacental transport of maternal immunoglobulin subclasses were comparable to the findings from previous reports, further demonstrating the reliability of this method. Therefore, our method provides a competitive approach to high-throughput detection of multiple immunoglobulin subclasses for biomonitoring or epidemiological studies.

CAS / MDL: 1066-33-7 144-48-9
研究领域: 免疫学 · 临床化学 · 妊娠研究 · 蛋白质组学
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Foods · 2025 ·Vol. 14 ·期 14 ·2490 · IF 5.1

Influences of Non-Volatile Components on the Aroma of Strong-Aroma Baijiu by Gas Chromatography-Olfactometry and Recombination-Omission Test

Yingqi Zhou,Yihong Wang,Jia Zheng,Siyi Pan,Xiaoyun Xu,Fang Yuan

Aroma is an important indicator for evaluating the quality of baijiu. In this study, we determined the aroma-active compounds in four representative brands of strong-aroma baijiu from Sichuan and Jianghuai regions through GC-MS/O, and GC-TOF-MS quantification. In addition, the non-volatile composition of four baijiu samples was quantified by BSTFA derivatization and GC-MS. By constructing a full recombination model containing both volatile and non-volatile components, the effect of different groups of non-volatile compounds on the aroma of strong-aroma baijiu was evaluated through recombination-omission tests. A total of 72 aroma-active compounds and 59 non-volatile compounds were identified and quantified. The results indicated that pyrazines, furfural, and furan derivatives displayed higher aroma intensities in strong-aroma baijiu produced in Sichuan compared to that produced in Jianghuai. The recombination model that included both aroma-active and non-volatile compounds showed a closer resemblance to the original baijiu samples, underscoring the critical role these compounds play in shaping the dominant aroma profile of strong-aroma baijiu. Non-volatile compounds significantly influenced six aroma attributes: fruity, sweet, sauce, pit, acidic, and alcoholic notes. Omission tests revealed that among posorly volatile organic acids, monobasic acids had distinct effects on the aroma profile, while dibasic acids did not show any noticeable influence on the sensory characteristics.

CAS / MDL: 64-17-5 75-09-2
研究领域: 食品科学 · 分析化学 · 风味化学 · 感官分析 · 酿造技术
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Analytical Methods · 2014 ·Vol. 6 ·期 13 ·4845-4852 · IF 1.938

UPLC-Q-TOF/MS characterization, HPLC fingerprint analysis and species differentiation for quality control of Nigella glandulifera Freyn et Sint seeds and Nigella sativa L. seeds

Qi Yun,Qingwang Liu,Cunyong He,Xiaohua Ma,Xiaoli Gao,Amer Talbi,Jianping Zhou

Nigella glandulifera Freyn et Sint seeds (NG) as well as Nigella sativa L. seeds (NS) have been employed as folk remedies for centuries. However, little work has been done on their quality control. In order to assess the quality and guarantee therapeutic effects, the chemical constituents of the two herbs were extensively characterized by ultra-performance liquid chromatography coupled with electrospray time-of-flight mass spectrometry (UPLC-Q-TOF/MS), and a simple, practical, and reliable HPLC fingerprinting method was established and applied to determination of 20 batches of samples. With their chromatographic fingerprints, the two species were successfully differentiated by pattern recognition methods, namely, principal component analysis (PCA) and partial least square discriminant analysis (PLS-DA). Results from this study show that the proposed analytical methods can be applied to the quality control of the seeds and have high potential to ensure their safety and efficacy.

CAS / MDL: 99-96-7 491-54-3 73-22-3
研究领域: 药用植物学 · 分析化学 · 药学
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JOURNAL OF CHROMATOGRAPHY A · 2023 · IF 4.1

Rapidly and accurately screening histidine decarboxylase inhibitors from Radix Paeoniae alba using ultrafiltration–high performance liquid chromatography/mass spectrometry combined with enzyme channel blocking and directional enrichment technique

Guizhou Hu,Lu Wang,Xinqi Li,Jin Qi

Histidine Decarboxylase (HDC), an unique enzyme responsible for the synthesis of histamine, which is an important mediator in allergy. Inhibition of HDC activity to decrease histamine production is one way to alleviate allergic symptoms. Traditional Chinese medicines (TCMs) with reported anti-allergy effect is one of important source to search for natural HDC inhibitor. Ultrafiltration combined with high–performance liquid chromatography/mass spectrometry (UF–HPLC/MS) is an effective method for screening HDC inhibitor from TCMs. Nevertheless, false-positive and false-negative results caused by the non-specific binding and the neglection of the trace active compounds are major problems in this method. In this study, an integrated strategy that combined UF–HPLC/MS with enzyme channel blocking (ECB) technique and directional enrichment (DE) technique was developed to seek natural HDC inhibitors from Radix Paeoniae alba (RPA), and at the same time, to reduce false-positive and false-negative results. HDC activity was detected to determine the validity of the screened compounds by RP–HPLC–FD in vitro . Molecular docking was applied to assay the binding affinity and binding sites. As a result, three compounds were screened from low content components of RPA after the DE. Among them, two non-specific compounds were eliminated by ECB, and the specific compound was identified as catechin, which has obvious HDC inhibition activity with IC 50 0.52 mM. Furthermore, gallic acid (IC 50 1.8 mM) and paeoniflorin (IC 50 >2 mM) from high content components of RPA were determined having HDC inhibitory activity. In conclusion, the integrated strategy of UF–HPLC/MS combined with ECB and DE technique is an effective mode for rapid and accurate screening and identification of natural HDC inhibitors from TCMs.

CAS / MDL: 64-19-7 643-79-8
研究领域: 药理学 · 分析化学 · 传统中药 · 过敏研究
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Journal of Environmental Chemical Engineering · 2024 · IF 7.4

Pyrene biodegradation by bacterial consortia enriched from coastal and marine sediments: Insights into bacterial community structures and functions

Huili Zeng,Jingyi Huang,Minghuo Wu,Minjie Hu,Xiaojing Yang,Hao Zhou,Jingjing Zhan,Xuwang Zhang

As a representative polycyclic aromatic hydrocarbon (PAH), pyrene poses a significant threat to the environment and public health due to its persistence and potential toxicity. Extensive research has been conducted on biodegradation of pyrene, highlighting the crucial need to unravel its degradation mechanisms. Coastal and marine sediments are promising sources for discovering microbial candidates capable of degrading pyrene. In this study, three bacterial consortia, designated as BS, YS, and SS, were enriched from sediments collected from the Bohai Sea, Yellow Sea, and Liao River estuarine wetland, respectively. The bacterial consortia BS, YS, and SS demonstrated high pyrene degradation efficiencies, achieving 86.61 %, 80.39 %, and 75.70 % degradation at the concentration of 50 mg/L within 8 days, respectively. High-throughput sequencing of 16S rRNA gene amplicons revealed Pandoraea , Delftia , and Pseudomonas as the dominant populations in bacterial consortia BS, YS, and SS, respectively, with some species potentially being novel pyrene degraders. Further analysis included identifying pyrene degradation metabolites by LC-Q-TOF-MS (high-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry) and predicting functional genes through PICRUSt (Phylogenetic Investigation of Communities by Reconstruction of Unobserved Stats). Based on these results, the metabolic pathways for pyrene degradation by the bacterial consortia were proposed, which predominantly involved the dioxygenation pathway. Overall, these findings should offer valuable bacterial resources for facilitating the bioremediation of PAH-contaminated environments.

CAS / MDL: 129-00-0
研究领域: 环境微生物学 · 生物修复 · 海洋生态学 · 分子生物学
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

New UHPLC-Q-Orbitrap MS/MS-based Library-comparison method simultaneously distinguishes 22 phytophenol isomers from Desmodium styracifolium

Xican Li,Jingyuan Zeng,Rongxin Cai,Chunhou Li

Isomers distinction has become a bottleneck of the emerging ultra-high-performance liquid chromatography coupled with hybrid quadrupole-orbitrap tandem mass spectrometry (UHPLC-Q-orbitrap MS/MS) technology. The present study thus used Desmodium styracifolium as model plant to establish a new library-comparison method for isomers distinction. The method firstly established a data library comprising MS/MS characteristic fragment, MS/MS profile, and retention time (R.T.) value. Through subsequent comparisons, 22 phytophenol isomers in D. styracifolium have been simultaneously distinguished under MS spectra negative model. The results suggested that: (1) there were four main types of isomers, i.e., positional isomers, functional group isomers, skeleton isomers, and hybridized isomers. (2) The hybridized isomers (e.g., luteoloside and astragalin) could be easily distinguished, while positional isomers (e.g., schaftoside and isoschaftoside) were difficultly distinguished from each other. (3) The R.T. value comparison played a key role for distinction of highly similar isomers, especially positional isomers. On the basis of above results and computational chemistry, it is concluded that, the new UHPLC-Q-orbitrap MS/MS-based library-comparison method can be capable for isomers distinction and thus has developed the UHPLC-Q-orbitrap MS/MS technology. The development will benefit many fields, including food, herbal medicine, and analysis chemistry. Particularly, the data of 22 phytophenol isomers can be directly cited for their isomersdistinction in future by other researchers.

CAS / MDL: 520-18-3
研究领域: 分析化学 · 天然药物化学 · 食品科学 · 中药学
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JOURNAL OF APPLIED POLYMER SCIENCE · 2023 · IF 3

A novel bio-based charcoal-forming agent based on chitosan and phytate@Mg to improve the flame retardancy of poly(lactic acid)

Yuhan Chen,Nian Yin,Yunfei Wang,Shanjun Gao,Chunhui Shen

A novel bio-based carbon forming agent (Mg@PA-CS) containing P and N elements was were synthesized using the complexation characteristics of chitosan (CS) and phytate (PA). The flame retardant behavior of poly(lactic acid) (PLA)/Mg@PA-CS/APP composites (addition of 20 wt% of different ratios of Mg@PA-CS and APP to polylactic acid composites) were investigated by the limiting oxygen index (LOI), vertical burning test (UL-94), cone calorimetry test (CCT), and thermogravimetric analysis (TGA). Due to the biphasic flame retardant and synergistic effect, since the 20 wt% flame retardant system (Mg@PA-CS:APP = 1:2), PLA composites passed the UL-94 test V-0 rating, reached 34% LOI value. The peak heat release rate (PHRR) and total heat release rate (THR) were reduced to 1/2 of the pure PLA, char residue could be as high as 11.49% at 800°C. Moreover, the flame-retardant mechanism of PLA composites during thermal decomposition was analyzed using a scanning electron microscope (SEM) and the coupling techniques of TGA linked with FT-IR (TG-FTIR).

CAS / MDL: 68333-79-9
研究领域: 材料科学 · 高分子科学 · 消防安全工程
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Oncotarget · 2017 · IF 5.168

Mass spectral analysis of the multikinase inhibitor BZG and its metabolites and analysis of their binding to vascular endothelial growth factor receptor-2

Yan Lou,Wenqi Qiu,Zhe Wu,Qian Wang,Yunqing Qiu,Su Zeng

We previously showed that BZG is a novel multitarget kinase inhibitor, which inhibited hepatocellular carcinoma in vivo and in vitro . In the present study, we used ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF MS) to characterize BZG and its metabolites generated in vivo . The probable metabolic mechanism was further confirmed by analysis of Phase I and Phase II metabolism in liver microsomes and with recombinant enzymes. In addition, the binding affinities of BZG metabolites to vascular endothelial growth factor receptor 2 (VEGFR2) were predicted using electronic high throughput screening (eHiTS). The results showed that BZG underwent phase I and phase II metabolism. We detected 11 BZG metabolites and identified hydroxylation, glucuronation, acetylation, sulfonation and degradation as the major metabolic processes in vivo and in vitro . Five of the eleven metabolites showed highly favorable eHiTS energy scores that were lower than sorafenib. Knowledge of the in vivo metabolic pathways of BZG and its binding affinities to VEGFR2 will be beneficial for further clinical development of BZG.

研究领域: 药理学 · 癌症研究 · 药物代谢
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TALANTA · 2016 · IF 4.035

Powder X-ray diffraction detection on a paper-based platform

Liangfei Ouyang,Qian Liu,Chaoping Xu,Changgui Liu,Heng Liang

We developed paper-based powder X-ray diffraction (PP-XRD) to implement phase identification and/or crystal structure determination on paper-based platforms. These aims are not possible with other paper-based detectors, such as Raman spectroscopy and mass spectrometry. PP-XRD overcomes these limitations. Here we reported the simple and low-cost in situ PP-XRD protocol for phase identifications of inorganic and organic materials. We demonstrated that sample amounts of lead nitrate on paper substrate can be reduced into 1/30 of conventional ones by using the standard glass substrate at the same signal-to-noise ratio (S/N) of the X-ray diffraction (XRD) pattern. The paper-based method was comparable in sample quantity and intensity with zero background holder method, even though single crystal Si(100) substrate as zero background holder was used for the specimen preparation of CTAB (C 19 H 42 BrN). More importantly, paper substrates helped reduce preferred orientation that was generally present in routine powder XRD. Also, combined with paper chromatography , overlap peaks were eliminated in the XRD detection patterns of lead nitrate and cobalt nitrate hexahydrate. This new PP-XRD protocol may accelerate the process to identify phase or determine the molecular structures of new materials using trace sample directly. It also includes a hyphenated technique of powder XRD with a simple paper-based microfluidic separation of chemical solutions .

研究领域: 材料科学 · 分析化学 · X射线衍射 · 基于纸的设备 · 微流控技术
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Advanced Healthcare Materials · 2024 · IF 10

A Sustainable Retinal Drug Co-Delivery for Boosting Therapeutic Efficacy in wAMD: Unveiling Multifaceted Evidence and Synergistic Mechanisms

Congyan Liu,Wenting Su,Xi Jiang,Yanli Lv,Fei Kong,Qin Chen,Qun Zhang,Huangqin Zhang,Yuping Liu,Xiaoqi Li,Xinrong Xu,Yan Chen,Ding Qu

Sustainable retinal codelivery poses significant challenges technically, although it is imperative for synergistic treatment of wet age-related macular degeneration (wAMD). Here, a microemulsion-doped hydrogel (Bor/PT-M@TRG) is engineered as an intravitreal depot composing of temperature-responsive hydrogel (TRG) and borneol-decorated paeoniflorin (PF) & tetramethylpyrazine (TMP)-coloaded microemulsions (Bor/PT-M). Bor/PT-M@TRG, functioning as the “ammunition depot”, resides in the vitreous and continuously releases Bor/PT-M as the therapeutic “bullet”, enabling deep penetration into the retina for 21 days. A single intravitreal injection of Bor/PT-M@TRG yields substantial reductions in choroidal neovascularization (CNV, a hallmark feature of wAMD) progression and mitigates oxidative stress-induced damage in vivo. Combinational PF&TMP regulates the “reactive oxygen species/nuclear factor erythroid-2-related factor 2/heme oxygenase-1” pathway and blocks the “hypoxia inducible factor-1α/vascular endothelial growth factor” signaling in retina, synergistically cutting off the loop of CNV formation. Utilizing fluorescence resonance energy transfer and liquid chromatography-mass spectrometry techniques, they present compelling multifaceted evidence of sustainable retinal codelivery spanning formulations, ARPE-19 cells, in vivo eye balls, and ex vivo section/retina-choroid complex cell levels. Such codelivery approach is elucidated as the key driving force behind the exceptional therapeutic outcomes of Bor/PT-M@TRG. These findings highlight the significance of sustainable retinal drug codelivery and rational combination for effective treatment of wAMD.

CAS / MDL: 38215-36-0
研究领域: 药学 · 眼科学 · 药物递送系统 · 生物医学工程
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