Analytical Methods
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2021
·Vol. 13
·期 11
·1412-1421
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IF 2.896
Wenjia Fan,Dan Yang,Nan Ding,Puyu Chen,Lei Wang,Guanwei Tao,Feng Zheng,Shunli Ji
Core–satellite-structured magnetic nanosorbents (MNs) used for the selective extraction of macrolide antibiotics (MACs) were prepared in this study. The MNs (core–satellite polydopamine-coated Fe3O4 nanoparticles–hollow porous molecularly imprinted polymer) consisted of polydopamine-coated Fe3O4 nanoparticles (Fe3O4@PDA) “core” linked to numerous hollow porous molecularly imprinted polymer (HPMIP) “satellites” with bridging amine functional groups. It is worth mentioning that HPMIPs act as “anchors” for selectively capturing target molecules. Polymers were characterized using TEM, SEM, FT-IR, VSM, and TGA and applied as magnetic dispersive solid-phase extraction (MDSPE) sorbents for the enrichment of trace MACs from a complex food matrix prior to quantification by HPLC-MS/MS. Nanocomposites revealed outstanding magnetic properties (36.1 emu g−1), a high adsorption capacity (103.6 μmol g−1), selectivity (IF = 3.2), and fast kinetic binding (20 min) for MACs. The multiple advantages of the novel core–satellite-structured magnetic molecularly imprinted nanosorbents were confirmed, which makes us believe that the preparation method of the core–satellite MNs can be applied to other fields involving molecular imprinting technology.
研究领域:
分析化学
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环境科学
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食品科学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2019
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IF 5.399
Zhong-Yuan Liu,Da-Yong Zhou,Ao Li,Man-Tong Zhao,Yuan-Yuan Hu,De-Yang Li,Hong-Kai Xie,Qi Zhao,Xiao-Pei Hu,Jiang-Hua Zhang,Fereidoon Shahidi
This study aimed at investigating the formation and accumulation of 16 reactive aldehydes in clam ( Ruditapes philippinarum ) during oil frying in both the tissue and the oil using an HPLC-ESI-MS/MS methodology. After processing, the accumulation of acrolein, crotonaldehyde, pentanal, trans -2-hexenal, hexanal, trans , trans -2,4-heptadienal, heptanal, nonanal, trans , trans -2,4-decadienal and 4-hydroxy-2-nonenal was most noticeable in both fried clam and frying oil. Most of the aldehyde species showed a time- and temperature-dependent manner of formation and accumulation during frying due to continuous oxidative degradation under conditions employed. However, several species of aldehyde such as acrolein and trans -2-pentenal slightly decreased at higher temperatures and/or longer frying times, which may be due to the imbalance toward disappearance of aldehydes resulting from their evaporation under the extreme conditions. Presence of natural polyphenols in bamboo leaves significantly prevented the formation of aldehydes in both fried clam and frying oil due to their antioxidant activity ( P < 0.05).
研究领域:
食品科学
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分析化学
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生物化学
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DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2020
·
IF 4.192
Wei Dong,Ruonan Guo,Wenxuan Lin,Miao Liu,Caihong Shen,Xiaotao Sun,Baoguo Sun,Bo Deng
Simultaneous detection of 3-indoleacetic acid (IAA) and 3-indolepropionic acid (IPA) in strong-aroma types of base Baijiu (base SAB) is crucial for elucidating the metabolic pathway of 3-methylindole during the base SAB brewing. Herein, a novel magnetic poly(allylamine)-modified graphene oxide (GO@PAA@Fe3O4) was synthesized as extraction sorbent, followed by high performance liquid chromatography mass spectrometry HPLC-MS/MS. As a surface modifier of GO, the introduction of PAA and Fe3O4 provided more adsorption sites for IAA and IPA, mainly through the generation of H-bonding sites. Moreover, modified by an activation step, the capacity of the activated GO@PAA@Fe3O4 for the adsorption of IAA and IPA was 2.1–3.4 times higher than that of unactivated material. The adsorptions of IAA and IPA on GO@PAA@Fe3O4 were fitted to the pseudo-second-order kinetic model and Langmuir isotherm, respectively. Under the optimal conditions, IAA and IPA were determined in 16-base SAB for the first time, and their concentrations ranged from 0.6 to 11.3 and 0.7 to 18.7 μg/L, respectively.
研究领域:
分析化学
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食品科学
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纳米技术
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2022
·
IF 3.318
Guiya Yang,Pai Liu,Huan Shi,Weixu Fan,Xie Feng,Jiabao Chen,Songsong Jing,Lei Wang,Yuguang Zheng,Dan Zhang,Long Guo
The rhizome of Dioscorea nipponica Makino (RDN) is a widely used herbal medicine, which has significant anti-inflammatory activities on various inflammatory diseases. However, the bioactive compositions responsible for the anti-inflammatory activity of RDN are still unknown. This study aimed to identify the anti-inflammatory bioactive compounds in RDN using high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-Q/TOF-MS), quantitative analysis of multiple components by single marker (QAMS) and chemometric methods. Firstly, an HPLC-Q/TOF-MS method was employed for identification of bioactive steroidal saponins in RND, and a total of twelve steroid saponins were identified. Then, QAMS method was employed to determine the contents of seven bioactive steroidal saponins, including protodioscin, protogracillin, methyl protodioscin, pseudoprotodioscin, pseudoprogracillin, dioscin and gracillin in RND samples using dioscin as the reference analyte. The anti-inflammatory effects of RDN samples were then evaluated by inhibition of NO production in LPS-induced RAW264.7 cells. Furthermore, chemometric methods, including Pearson correlation analysis and partial least squares regression (PLSR) were employed to investigate the correlations between chemical components and anti-inflammatory activities, and explore the potential anti-inflammatory bioactive compounds of RDN. The results indicated that protodioscin, dioscin and gracillin were selected as the major anti-inflammatory compounds in RND. The further verification experiments showed that protodioscin, dioscin and gracillin exhibited great inhibition on NO production with IC 50 values (the half maximal inhibitory concentration) of 0.712 μM, 0.469 μM and 0.815 μM, respectively. They also significantly reduced the levels of TNF-α, IL-1β, and IL-6 in LPS-induced RAW264.7 cells. The present study provided evidences for the anti-inflammatory activity of RND and identification of the anti-inflammatory components in RDN.
研究领域:
生药学
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药物分析
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药理学
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分析化学
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生物化学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Ruidong Zhou,Cong Kong,Yupeng Wen,Guangxin Yang,Wendi Huo,Chaoying Zhang,Huiwu Sun,Huan Liu,Dongmei Huang,Jincheng Li
A 15-channel pressure filtration purification method was presented for high throughput sample preparation of aquatic products. A cost-effective device was constructed and melamine sponge was selected as the cleanup sorbent. Upon interfacing with HPLC-MS/MS, the analytical procedure demonstrated its suitability for quantifying 160 pesticides and veterinary drug residues in aquatic products such as fish, shrimp, and crab. The method achieved sample recoveries ranging from 61.3 to 124.9 %. The detection limits were established between 0.5 and 1.0 μg/kg, while the quantitation limits were confirmed to be within the range of 1.0–2.0 μg/kg. The method was applied to quantify the pesticide and veterinary drug residues in mostly consumed aquatic products from five coastal provinces in China. The results showed significant differences between different aquatic products in the concentrations of pesticide and veterinary drug residues, implying the necessity of supervision for the accurate determination of pesticides and veterinary drugs.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
TUBERCULOSIS
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2017
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IF 2.873
Shouhong Gao,Zhipeng Wang,Xinfang Xie,Chunhua You,Yang Yang,Yanhai Xi,Wansheng Chen
First-line anti-tuberculosis drugs are playing vital roles for curbing rapid spread of tuberculosis. Multidrug therapies are commonly applied in clinical to achieve better treatment outcomes. However, drug resistance and adverse reactions come along with this therapies and therapeutic drug monitoring is a feasible way to precaution them. For this reasons, a simple and sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and single protein precipitation was developed and validated for simultaneously quantifying of pyrazinamide, isoniazid, ethambutol , streptomycin and rifampicin in human plasma. Optimized chromatographic separation was achieved on a ZORBAX SB-C 18 column with heptafluorobutyric acid, an ion-pair reagent, in the mobile phase at a flow rate of 0.3 mL/min. The mass detection was achieved using electrospray ionization in the positive ion mode with a multiple reaction monitoring mode. The lower limit of quantification (LLOQ) and dynamic range of pyrazinamide, isoniazid, ethambutol, streptomycin and rifampicin were 200–4000 ng/mL, 80–2000 ng/mL, 0.2–1000 ng/mL, 2000–200000 ng/mL and 200–4000 ng/mL, respectively. The Inter-day and intra-day accuracy and precision were within ±15.0% and less than 15%. The method had been successfully applied to simultaneous determination of four first-line Anti-tuberculosis drugs in plasma from tuberculosis patients.
研究领域:
临床医学
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药理学
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分析化学
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DOI
PubMed
高影响因子
Food Bioscience
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2024
·
IF 4.8
Jing Guo,Xiaojie Yu,Cunshan Zhou,Bo Wang,Lei Zhang,Phyllis Otu,Li Chen,Yunwei Niu,Deyang Yao,Chenhui Hua,Haile Ma
Gradient dilution feeding substrate (GDFS) is regarded as an effective method for the production of active peptides, as it compensates for substrate limitations and minimizes substrate contamination of the ultrafiltration membrane. This study further investigated the impact of ultrasound-assisted gradient dilution feeding substrate (UA-GDFS) on the peptide yield and the intensity of umami. The chicken breast was used as ingredients. The umami compounds in the hydrolysate were determined using an automatic amino acid analyzer and HPLC. The hydrolysate's umami intensity was determined by electronic tongue in all modes. These findings indicated that UA-GDFS enhanced the umami intensity and peptide yield. Hydrolysate from UA-GDFS with molecular weight below 1 kDa was analyzed by nano-scale liquid chromatography-tandem mass spectrometry (Nano-HPLC-MS/MS). Electronic tongue analysis showed that GPSGPVG and VDGPSGK had umami taste and could enhance the umami taste of monosodium glutamate (MSG) solution. Asn68 and His145 were important sites on T1R3 for umami peptide binding.
研究领域:
食品科学
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化学工程
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分析化学
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产品关联
DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
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2021
·
IF 4.952
Zheng Zhou,Yu-Ying Zhang,Jing-Xuan Gao,Li-Xin Ma,Xu-Hui Huang,Jie Zheng,Xiu-Ping Dong,Lei Qin
This study investigated the changes in free amino acids (FAAs), 5′-nucleotides, and lipid compositions of Manila clams ( Ruditapes philippinarum ) collected from December 2017 to November 2018. High-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry was used to quantify twenty-one FAAs and six 5ʹ-nucleotides. Lipid profiles were explored by ultra-performance liquid chromatography coupled with a Q-Exactive Orbitrap mass spectrometer with an untargeted lipidomic approach. Results showed significant monthly changes of FAAs, 5′-nucleotides, and lipids profiles. Alanine , glutamic acid , glycine, and aspartic acid , which contributed to the sweet and umami flavor, were the most abundant FAAs in Manila clams. Totally 90 glycerides, 76 glycerophospholipids , 21 lyso-glycerophospholipids, and 52 fatty acids were identified in Manila clams. Among these lipids, most of them possessed a high-level of unsaturation degree. The unsaturation degree of lipids in February, March, and April was the highest, showing the best nutritional value of Manila clams.
研究领域:
海洋生物学
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代谢组学
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食品科学
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营养学
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DOI
高影响因子
ACS Omega
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2022
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IF 4.132
Lei Zhu,Li Liu,Le Du,Jingmei Hao,Jianhua Ma,Jun Zhu,Wenjing Gong
A rapid, accurate, and selective analytical method to simultaneously quantify 13 anticoagulant rodenticides in animal biological samples was developed using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) coupled with electrospray ionization (ESI) in negative mode. Samples were extracted and purified based on a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) sample preparation technique. The sample pH and the type of extraction solvent and cleanup sorbent used to estimate the procedure’s effectiveness were optimized. To improve the matrix effects and obtain acceptable recoveries for 13 rodenticides, 0.1 mL/g biological sample and 1 mL acetonitrile (or acetonitrile: EtOAc = 1:1/(v:v)) extraction followed by Florisil/HC-C18/anhydrous Na2SO4 (NaCl) cleanup under alkaline conditions was fully validated and shown to be selective, precise, accurate, and linear in the range from 1 to 100 ng/mL (g). The mean recoveries were between 52.78 and 110.69%, while the limits of detection and quantification ranged from 0.05 to 0.5 and 0.1–1 ng/mL (μg/kg), respectively. Ideal soft matrix effects (≤20%) were observed for the vast majority of rodenticides (>95%) showing either suppression or enhancement. This method meets international criteria and is capable of simultaneously identifying and quantifying anticoagulant rodenticides in animal blood and tissues and can be suitable for the detection of poisoning cases in the field of forensic or public health.
研究领域:
分析化学
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毒理学
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法医学
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公共卫生
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DOI
PubMed
高影响因子
MOLECULES
·
2026
·Vol. 31
·期 11
·1780
·
IF 5.1
Xiaohui Cai,Jun Men,Qingwu Yang,Yili Hu,Zhixian Qiao
A derivatisation-free HPLC–MS/MS method was developed and validated for the simultaneous quantification of selenium- and sulphur-containing amino acids in soybean leaves, and applied to a 3 × 3 factorial hydroponic experiment probing selenium–sulphur metabolic interactions. The method resolves five biologically informative analytes (Cys2, SeCys2, MeSeCys, Met, SeMet) within 1.5 min through multiple reaction monitoring (MRM). Ultrasound-assisted extraction (UAE) of the free fraction was jointly optimised for both analyte classes by the response-surface methodology; enzymatic hydrolysis of the extraction residue recovered the protein-bound fraction on the same platform. Limits of detection ranged from 0.036 to 0.556 µg L−1, intra-day relative standard deviations were below 5%, and spike recoveries fell between 92.3 and 117.4%. Free SeAA and SAA pools were negatively correlated across the nine treatments (R2= 0.83), consistent with competitive Se–S assimilation, whereas bound pools were positively correlated (R2= 0.89), reflecting proportional protein-level incorporation. A regime of 1–5 mM of sulphate with 20 µM of selenite yielded the highest bound organo-Se with near-normal growth, providing leaf-level evidence that may inform future seed-focused studies aimed at Se-enriched soy-protein ingredient development.
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DOI
PubMed
高影响因子
Drug Design Development and Therapy
·
2026
·
IF 6.1
Shengnan Wang,Shijia Lu,Guofei Li,Yingjie Qi
Purpose Hepatocellular carcinoma (HCC) is a highly lethal malignancy with poor prognosis and limited clinical treatments. CD8⁺ T cell-based immunotherapy offers promising therapeutic potential against HCC. We fabricated MMP-9/pH dual-sensitive liposomes co-encapsulating enzalutamide, GB-1107 and BMS-1166 for HCC treatment. Reliable detection approaches are lacking to assess in vivo liposomal behavior. This study established an HPLC-MS/MS method for simultaneous determination of the three drugs in rat plasma, and applied it to characterize their pharmacokinetic profiles.Methods The pH/MMP-9 dual-sensitive liposomes co-loaded with BMS-1166, GB-1107 and enzalutamide were prepared via the thin-film hydration method, and the resultant formulations exhibited satisfactory pharmaceutical properties meeting the predefined quality criteria. For chromatographic separation, a poroshell 120 EC-C18 column (50 × 4.6 mm, 2.7 μm) was adopted, combined with linear gradient elution of 0.1% formic acid in water and acetonitrile. Full validation of the established method was performed strictly following the guidelines for bioanalytical method validation as stated in the Chinese Pharmacopoeia.Results BMS-1166, GB-1107, and enzalutamide exhibited good linearity over the concentration range of 1.0–1000.0 ng/mL. The accuracy and precision of BMS-1166, GB-1107, and enzalutamide all fall below 11.1%. In addition, the recoveries and matrix effect for these analytes ranged from 88.6%-99.7%. Pharmacokinetic results demonstrated that the prepared liposomes possessed favorable in vivo long-circulating properties, which prolonged the half-lives of BMS-1166 and GB-1107 by 25-fold and 13-fold, respectively, and enhanced their bioavailability by 35-fold and 30-fold, respectively. In contrast, no statistically significant effect was observed on enzalutamide.Conclusion The established method was validated and met the predefined quality criteria, thereby being suitable for investigating the in vivo pharmacokinetic profiles of BMS-1166, GB-1107, and enzalutamide.
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PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2025
·
IF 11.3
Wendi Huo,Jincheng Li,Yupeng Wen,Xinyuan Zhang,Huan Liu,Yingchun Mu,Chunhui Zhao,Chaoying Zhang,Rongyue Zhang
In this study, we present a simple and rapid boronate affinity extraction methodology for the HPLC-MS/MS analysis of four nitrofuran metabolites (NFMs) including SEM, AOZ, AHD and AMOZ in fish samples. To enhance the efficacy of this approach, mesoporous poly(GMA-EGDMA) microspheres, abundant in cis-diols, were synthesized for boronate affinity extraction. Meanwhile, 4-fluoro-3-formylphenyl boronic acid was utilized for the derivatization of NFMs, facilitating the immobilization of boronate ligands onto their molecular structures. Compared to the Chinese national food safety standard GB 31656.13–2021, the boronate affinity extraction eliminates the need for extraction solvents and centrifugation, streamlines the pretreatment process, and maintains a mild extraction environment. Furthermore, the poly(GMA-EGDMA) microspheres exhibited excellent reusability, retaining their performance over six adsorption-desorption cycles. The NFMs demonstrated excellent linearity (R² > 0.999) across the range of 0.5 to 50 µg kg⁻¹ . The quantitative limit was established at 0.5 µg kg⁻¹ . The recoveries of spiked tilapia samples ranged from 94.2 % to 110.7 %, while intra-day and inter-day RSDs were below 5.9 %. This method emerges as an economical, straightforward, rapid, and sensitive alternative for monitoring of NFM residues in aquatic products.
研究领域:
食品科学
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分析化学
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环境科学
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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）