JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2024
·
IF 4
Ming Yang,Jun Yi,Yuan Yang,Han Xiao,Jia Xu
A solid-phase extraction (SPE) method using three-dimensional covalent organic framework (COFs) coupled with ultra-high performance liquid chromatography-mass spectrometry was developed for the detection of 13 fluoroquinolones (FQs) in bean sprout samples. Critical extraction parameters influencing SPE efficiency were optimized and matrix-matched standard curves were used to eliminate matrix effects and validate the proposed method. The analytical method proved to have good linearity in the concentration range of 1.0–100 μg L –1 with correlation coefficients of r≥0.9995. The limits of detection were 0.10–0.45 μg kg –1 , whereas the limits of quantification were 0.34–1.51 μg kg –1 . The recoveries ranged from 92.7 % to 105 % with satisfactory precision (< 4.82 %). The COFs-packed SPE cartridge maintained recovery efficiency for the target FQs over five reuse cycles. The adsorption selectivity was mainly attributed to π–π interactions, hydrogen bonding, and electrostatic attraction between FQs and the adsorbent. Analysis of actual samples revealed the presence of enrofloxacin, ciprofloxacin, and norfloxacin in three batches of bean sprout samples. These results highlight the importance of monitoring antibiotics residues in bean sprouts.
研究领域:
分析化学
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食品科学
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环境科学
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高影响因子
Foods
·
2024
·Vol. 13
·期 20
·3286
·
IF 4.7
Di Huang,Chengbin Liu,Huatian Zhou,Xianli Wang,Qicai Zhang,Xiaoyu Liu,Zhongsheng Deng,Danhe Wang,Yameng Li,Chunxia Yao,Weiguo Song,Qinxiong Rao
This study established novel and high-throughput strategies for the simultaneous analysis of 30 fluorinated emerging pollutants in different matrices from the shrimp aquaculture system in eastern China using UHPLC-MS/MS. The parameters of SPE for analysis of water samples and of QuEChERS methods for sediment and shrimp samples were optimized to allow the simultaneous detection and quantitation of 17 per- and polyfluoroalkyl substances (PFASs) and 13 fluoroquinolones (FQs). Under the optimal conditions, the limits of detection of 30 pollutants for water, sediment, and shrimp samples were 0.01–0.30 ng/L, 0.01–0.22 μg/kg, and 0.01–0.23 μg/kg, respectively, while the limits of quantification were 0.04–1.00 ng/L, 0.03–0.73 μg/kg, and 0.03–0.76 μg/kg, with satisfactory recoveries and intra-day precision. The developed methods were successfully applied to the analysis of multiple samples collected from aquaculture ponds in eastern China. PFASs were detected in all samples with concentration ranges of 0.18–0.77 μg/L in water, 0.13–1.41 μg/kg (dry weight) in sediment, and 0.09–0.96 μg/kg (wet weight) in shrimp, respectively. Only two FQs, ciprofloxacin and enrofloxacin, were found in the sediment and shrimp. In general, this study provides valuable insights into the prevalence of fluorinated emerging contaminants, assisting in the monitoring and control of emerging contaminants in aquatic foods.
研究领域:
环境科学
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分析化学
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水产养殖学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2025
·
IF 5.1
Xinyuan Pei,Nan Zhang,Yuting Chen,Shiyu Miao,Huiyang Fu,Qingqing Zhu,Zhengbo Dai,Yi Chi,Ligang Hu,Rong Jin,Chunyang Liao
Antibiotics, as a typical class of emerging contaminants in the environment, are frequently detected at trace concentrations in various water samples. The chemical properties of antibiotics exhibit significant diversity, encompassing variations in molecular structure, amphoteric behaviour, and polarity. These differences present substantial challenges in developing universal detection methods for comprehensive monitoring of antibiotic contaminants. Therefore, it is imperative to develop more targeted, efficient, and sensitive analytical techniques. In this study, we develop a solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method. This method enables the simultaneous determination of 69 antibiotics divided into seven categories (tetracyclines, quinolones, sulfonamides, β-lactams, macrolides, lincosamides, and chloramphenicols) in surface water. The method achieved limits of detection (LOQs) ranging from 0.002 to 1.71 ng/L. The standard curves of the target compounds exhibited excellent linearity, with correlation coefficients (r 2 ) > 0.995, and most spiked recoveries fell within the range of 40.4–149 %, with relative standard deviations (RSDs) below 15 %. Using this method, 19 surface water samples from Qiantang River Basin, Zhejiang Province, China were analyzed, with 29 out of 69 analytes being detected (the total concentrations ranging from 5.69 to 131 ng/L). This method provides a reliable and robust analytical approach for the comprehensive monitoring of antibiotic contaminants in environmental water, offering critical insights for pollution control and water quality management efforts.
研究领域:
环境科学
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分析化学
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高影响因子
Food Frontiers
·
2024
·Vol. 5
·期 3
·1004-1013
·
IF 7.4
Di Yuan,Yuting Yuan,Liangxiao Zhang,Fei Ma,Peiwu Li
A fast, simple, and sensitive analytic method was proposed for the simultaneous quantification of aflatoxins (AFTs) and capsaicinoids in vegetable oils by immunomagnetic sorbent coupled with ultra-performance liquid chromatography coupled with tandem mass spectrometry. The immunomagnetic solid phase extraction (IMSPE) sorbents were synthesized with the monoclonal antibodies via cyanogen bromide magnetic sorbents, which could modify the surface magnetic sorbents under mild synthetic condition. The IMSPE procedure had the following aspects such as ease manipulation, easy disperse, quick isolation, eco-friendly, and cost-effective. The major conditions of IMSPE procedure were systemically studied, and the optimized pretreatment was accomplished in 15 min avoding complicated condition or sophisticated equipment. Excellent linearities were achieved by the correlation ( R 2 ) more than 0.9983. The limits of quantifications of all analytes ranged from 0.03 to 0.20 µg kg −1 , and the recoveries were satisfactory ranging from 75.7% to 124.0% with the intra-day and inter-day precisions less than 10.1%. Additionally, the proposed method was used to analyze AFTs and capsaicinoids in retail oil samples. Overall, 25% of soybean and peanut oils and 12.5% of corn and blended oil were detected with AFTs, and no capsaicinoid was found. The content of AFTs was under the MRLs set by EU and China regulation for food quality and safety. The validated results indicated that this method could be utilized for a rapid, efficient, and accurate quantification of AFTs and capsaicinoids in complex lipid-based matrix.
研究领域:
食品安全
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分析化学
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生物技术
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DOI
高影响因子
Oil Crop Science
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2026
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IF 4.4
Jianzhou Qi,Fengwei Yang,Jixiang Hou,Liangxiao Zhang,Li Yu,Fei Ma,Peiwu Li
A simple, rapid and accurate method was developed to quantify DAGs by UHPLC-MS/MS. • Florisil SPE sorbent was used to extract and purify DAGs in lipid samples. • The SPE procedure could be achieved in 30 min with less volume of organic solvents. • All anaytes were chemical labelled under mild conditions with high efficiency. • The proposed method was used for the determination of DAGs in complicated matrices. s In the present study, a simple, accurate and simultaneous determination of diacylglycerol (DAG) compounds in vegetable oils were proposed by solid-phrase extraction (SPE) coupled with chemical labelling-based UHPLC-MS/MS. The experimental conditions of SPE purification, chemical labelling and UHPLC-MS/MS were investigated. Under the optimized parameters, the limit of quantification ranged from 4 μg kg -1 to 25 μg kg -1 , and the limit of detection ranged from 1 μg kg -1 to 7 μg kg -1 . Acceptable recoveries of all analytes were obtained ranging from 67.4% to 106.1% with the intra-day and inter-day precisions less than 14.8%. The validation results indicated that nine 1,3-DAG compounds were found at the concentration ranging from trace level to relative high amount in four types of edible oils. The proposed method simultaneously analyzed 16 DAG compounds in complicated matrix and accurately profiled the content and distribution of functional components in vegetable oils. Download: Download high-res image (128KB) Download: Download full-size image
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高影响因子
JOURNAL OF SEPARATION SCIENCE
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2026
·Vol. 49
·期 4
·e70409
·
IF 3.6
Xinyue Zheng,Yue Deng,Si Cheng,Di Lu,Yibo Wang,Zichang Tian,Hongyu Xue,Lei Yin,Meiyun Shi
In this study, a highly sensitive and selective ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed for the quantification of juglone, a poorly ionizable naphthoquinone, in biological matrices. To enhance ionization efficiency, pre-column derivatization was employed using sulfhydryl nucleophiles (β-mercaptoethanol and 3-mercaptopropionic acid) via Michael addition. Derivatization with mercaptopropionic acid significantly improved mass spectrometric response (50-fold increase) and minimized matrix effects compared to mercaptoethanol. The method, validated per FDA guidelines, exhibited excellent linearity ( r ≥ 0.995) from 3 to 150 ng/mL, with accuracy within −10.6% to 4.3% and precision between 1.29% and 5.34%. The lower limit of quantification was 3 ng/mL. Extraction recovery and matrix effects ranged from 99.84% to 102.06% and 92.75% to 98.98%, respectively, with derivatives demonstrating good stability. Cellular uptake studies in MCF-7 cells revealed time-dependent but limited intracellular accumulation of juglone, with the majority retained in the culture medium. This robust derivatization-based UHPLC–MS/MS approach provides a reliable tool for investigating juglone's pharmacokinetics and toxicological mechanisms.
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PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2026
·
IF 6.7
Yehua Yang,Jiaqi Li,Xuejin Li,Qichang Huang,Weiwei Jiang,Wei Zhang,Yuqian Jiang,Yao Tang
Phyllanthus emblica L. is a fruit with high medicinal and edible value. Its main bioactive component, gallic acid (GA), is significantly increased by hot air drying, yet the underlying chemical mechanism remains unclear. This study investigated the temperature-dependent transformation of phenolics during drying (80–130 °C) using UHPLC-MS/MS and Global Natural Products Social Molecular Networking (GNPS). High-temperature drying (110 to 130 °C) increases the GA content by 13.4–26.9 fold. Integrated metabolomic analysis suggests this accumulation results primarily from two nonenzymatic pathways: the thermal hydrolysis of glucose galloyl derivatives (e.g., glucogallin, digalloylglucose, and trigalloylglucose), and the degradation of glucuronic acid galloyl derivatives (e.g., 2-O-galloylgalactaric acid and monogalloylgalactonolactone). While temperatures >110 °C maximize gallic acid yield, the Maillard reaction products (e.g., 5-HMF) were also promoted. These findings elucidate the chemical mechanism of GA accumulation via ester bond cleavage, providing a scientific basis for optimizing drying protocols to balance medicinal quality and safety.
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PubMed
高影响因子
JOURNAL OF FOOD SCIENCE AND TECHNOLOGY-MYSORE
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2025
·
IF 3.3
Xu Yinshuo,Han Zai-Gang,Zhang Minghui,Shi Qing,Min Jun Zhe
Chinese Korean ethnic rice wine (CKRW), a traditional fermented wine made from rice or corn, has antioxidant and antihypertensive activities. There is no report on the study of α-Dicarbonyl compounds (α-DCs) in CKRW currently. The sensitive UHPLC-MS/MS method based on a novel derivatization reagent 3-benzyl-2-oxo-4λ3-thiazolidine-4-carbohydrazide (BOTC). It was used to label three α-DCs, including glyoxal (GO), methylglyoxal (MG) and 3-deoxyglucoside (3-DG) in rice wine. The calibration curves obtained good linearity (R 2 > 0.9997) and a relatively wide range of concentrations from 0.39 to 62.5 µM. LOD were 25–50 fmol. GO, MG, and 3-DG were detected in CKRW for the first time. Then, ten kinds of rice wine were purchased from five suppliers for quantitative comparison. At the result, the contents of the three α-DCs had differences in these wines. 3-DG was higher than the other two α-DCs. The method provided a reference for the detection of α-DCs in other fermented alcoholic drinks. Graphical abstract
研究领域:
食品化学
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分析化学
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发酵饮料
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代谢组学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
·
IF 3
Dan Xiao,Ying Jin,Mengyu Zhang,Xiangjie Di,Lisha Fu,Changke Jiang,Zhuoli Lai,Yating Ge,Shanmian Ji,Yuming Zhang,Li Zheng,Zhenlei Wang,Fang Gong
Persistent patent ductus arteriosus (PDA) is generally observed in preterm neonates. Oral ibuprofen is the standard treatment for closing PDA in China. To investigate the chiral pharmacokinetics of ibuprofen enantiomers in Chinese premature infants with PDA, a simple, fast, and sensitive analytical enantioselective technology was developed with ultra-performance liquid chromatography (UPLC) – tandem mass spectrometry (MS/MS). Chromatographic separation of (R)-ibuprofen and (S)-ibuprofen was accomplished on a Lux® 3 µm Cellulose-3 (150 mm × 2.0 mm, 3 μm) at a flow rate of 0.2 mL/min within 6 min. UPLC separation was achieved by isocratic elution with a mobile phase consisting of formic acid:water (75:1000000, v/v) and acetonitrile:methanol (1:1, v/v). Only 50 µL of plasma samples were pre-treated with acetonitrile precipitation. Ibuprofen-d 3 was used as an internal standard. The standard curves of both enantiomers were linear over a concentration range of 0.0500 μg/mL to 50.00 μg/mL. The method has been validated for selectivity, carryover effect, lower limit of quantification, precision, accuracy, matrix effect, extraction recovery, dilution integrity, and stability based on the existing guidelines of the National Medical Products Administration, the United States Food and Drug Administration, and the European Medicines Agency. This method has been successfully applied to investigate the pharmacokinetics of ibuprofen enantiomers in 9 preterm infants with PDA. Our results showed that a high chiral inversion ratio of (R)- to (S)-ibuprofen exists in Chinese preterm neonates. Further studies should be conducted to monitor drug concentration following oral administration of ibuprofen and to consider the effect of individual variations and ethnic differences in metabolizing enantiomers of ibuprofen in premature neonates with PDA.
研究领域:
药理学
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新生儿医学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yamin Liu,Xunjiang Wang,Jiaojiao Wei,Kangning Fu,Yilin Chen,Linnan Li,Zhengtao Wang,Li Yang
The severe respiratory dysfunctions associated with acute lung injury (ALI) and its sequelae have a high morbidity and mortality rate, are multifactorial, and lack a viable treatment. Considering the critical function that amino acids and derivatives play in the genesis of illnesses and the regulation of metabolic processes, monitoring the levels of metabolites associated with amino acids in biological matrices is necessary and interesting to study their pathological mechanisms. Exploring the dynamics of amino acid and derivatives levels and searching for biomarkers provides improved clinical ideas for the diagnosis and treatment of ALI. Therefore, we developed an ultra-high-performance liquid chromatography-electrospray tandem mass spectrometry (UHPLC-MS/MS) method that can simultaneously determine the amino acid and derivatives metabolic levels to study amino acid profiles in different biological samples to facilitate clinical research of ALI. In this study, 48 amino acids and derivatives, including neurotransmitters, polyamines, purines, and other types, were quantified simultaneously in a fast, high-throughput, sensitive, and reliable manner within a 15-minute run time without derivatization. No relevant studies have been reported to quantify these 48 amino acid metabolites in three biological samples simultaneously. Satisfactory linearity (R > 0.995), inter-day and intra-day accuracy (85.17–112.67% and 85.29–111.60%, respectively), inter-day and intra-day precision (RSD < 13.80% and RSD < 12.01%, respectively), matrix effects (81.00%–118.00%), recovery (85.09%–114.65%) and stability (RSD < 14.72%) were all demonstrated by the optimized method's successful validation for all analytes. In addition, the suggested method was effectively implemented in plasma, urine, and lung tissue from normal mice and mice with ALI, with the aim of finding potential biomarkers associated with ALI. Potential biomarkers were screened through multivariate statistical analysis and volcanic map analysis, and the changes of markers in ALI were again identified through heat map analysis and correlation analysis with biochemical indicators, which provided ideas and references for subsequent mechanism studies. Here, the technique created in this work offers a quick and dependable way to perform an integrated analysis of amino acids in a variety of biological materials, which can provide research ideas for understanding the physiopathological state of various diseases.
研究领域:
肺病学
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分析化学
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代谢组学
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临床研究
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生物化学
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DOI
PubMed
高影响因子
Pharmaceutics
·
2022
·Vol. 14
·期 5
·1071
·
IF 6.525
Lara Soares Aleixo de Carvalho,Vinícius Carius de Souza,Vinícius C. Rodrigues,Aline Correa Ribeiro,Jorge Willian Leandro Nascimento,Priscila V. S. Z. Capriles,Priscila de F. Pinto,Josué de Moraes,Ademar Alves da Silva Filho
Schistosomiasis, caused by parasites of the genusSchistosoma, is a neglected disease with high global prevalence, affecting more than 240 million people in several countries. Praziquantel (PZQ) is the only drug currently available for the treatment.S. mansoniNTPDases (known as SmNTPDases, ATP diphosphohydrolases orecto-apyrases) are potential drug targets for the discovery of new antischistosomal drugs. In this study, we screen NTPDases inhibitors fromCentella erecta(Apiaceae) using an ultrafiltration combined UHPLC-QTOF-MS method and potato apyrase, identifying asiaticoside as one of the apyrase-binding compounds. After isolation of asiaticoside fromC. erectaextract, we assessed its in vivo antischistosomal activities againstSchistosoma mansoniworms and its in vitro enzymatic apyrase inhibition. Also, molecular docking analysis of asiaticoside against potato apyrase,S. mansoniNTPDases 1 and 2 were performed. Asiaticoside showed a significant in vitro apyrase inhibition and molecular docking studies corroborate with its possible actions in potato apyrase andS. mansoniNTPDases. In mice harboring a patentS. mansoniinfection, a single oral dose of asiaticoside (400 mg/kg. p.o.) showed significantly in vivo antischistosomal efficacy, markedly decreasing the total worm load and egg burden, giving support for further exploration of apyrase inhibitors as antischistosomal agents.Keywords:Schistosoma mansoni;natural products;asiaticoside
研究领域:
药理学
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寄生虫学
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天然产物研究
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PubMed
高影响因子
Separation Science Plus
·
2026
·Vol. 9
·期 5
·e70227
·
IF 2.7
Qingqing Xiao,Chengsi Cao,Zuding Wang,Fei-fei Wang,Shizhi Jiang,Ting Lei
Pinus yunnanensis cones are a rich source of bioactive compounds; yet, the systemic exposure and mechanistic basis of their anti-breast cancer activity remain unclear. Herein, we systematically identify the systemically absorbed components of P. yunnanensis cone extract and elucidate its anti-breast cancer mechanisms using an integrated analytical and computational approach. An optimized ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed to overcome severe matrix interference and insufficient sensitivity, facilitating the rapid identification of active constituents in the crude extract. UHPLC–MS/MS-based analysis of rat plasma and feces revealed 16 (14 prototypes and 2 metabolites) and 12 (10 prototypes and 2 metabolites) systemically absorbed components, respectively, derived from 28 identified compounds. Subsequent network pharmacology combined with molecular docking validation was used to screen the anti-breast cancer active components, core targets, and key pathways. Integrated network pharmacology predicted coniferaldehyde, phyllanflexoid A, 3′,4′,5,5′,6,7-hexamethoxyflavone, dihydrocaffeic acid, usnic acid, and 7-oxodehydroabietic acid, as core components, targeting TP53, STAT3, PIK3R1, SRC, and PIK3CA and involving key pathways such as VEGF signaling pathway, aldosterone-regulated sodium reabsorption, prolactin signaling pathway, PD-L1/PD-1 checkpoint pathway in cancer, and ErbB signaling pathway. This study establishes a robust UHPLC–MS/MS platform for the quality control of P. yunnanensis cones and provides critical insights into their translational potential for anti-breast cancer drug development and advancing separation science applications in natural product research.
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高影响因子
危险品化学品经营许可证（带存储）