Journal of Pharmaceutical Analysis
·
2020
·
IF 2.673
Siqi Ren,Jingjing Liu,Yunwen Xue,Mei Zhang,Qiwei Liu,Jie Xu,Zunjian Zhang,Rui Song
Saikosaponins (SSs) are the main active components extracted from Bupleuri Radix (BR) which has been used as an important herbal drug in Asian countries for thousands of years. It has been reported that the intestinal bacteria plays an important role in the in vivo disposal of oral SSs. Although the deglycosylated derivatives (saikogenins, SGs) of SSs metabolized by the intestinal bacteria are speculated to be the main components absorbed into the blood after oral administration of SSs, no studies have been reported on the characteristics of SGs for their intestinal absorption, and those for SSs are also limited. Therefore, a rapid UHPLC-MS/MS method was developed to investigate and compare the apparent permeability of three common SSs (SSa, SSd, SSb 2 ) and their corresponding SGs (SGF, SGG, SGD) through a bidirectional transport experiment on Caco-2 cell monolayer model. The method was validated according to the latest FDA guidelines and applied to quantify the six analytes in transport medium samples extracted via liquid-liquid extraction (LLE). The apparent permeability coefficient ( P app ) determined in this study indicated that the permeability of SGs improved to the moderate class compared to the corresponding parent compounds, predicting a higher in vivo absorption. Moreover, the efflux ratio (ER) value demonstrated an active uptake of SSd and the three SGs, while a passive diffusion of SSa and SSb 2 .
研究领域:
药理学
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药剂学
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分析化学
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中药学
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PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2022
·Vol. 45
·期 15
·2977-2986
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IF 3.614
Minhan Huang,Ting Zhou
Pseudotargeted analysis combines the advantages of untargeted and targeted metabolomics methods. This study proposed a comprehensive pseudotargeted metabolomics method based on two-phase liquid extraction using ultra-high-performance liquid chromatography-tandem mass spectrometry. Two-phase liquid extraction, composed of both aqueous and organic phases, extracted a wide range of metabolites from polar to nonpolar in plasma samples. Besides, the two phases were combined and detected in a single injection to save analytical time. A total of 486 potential metabolites were detected by the developed approach. Compared with the conventional methanol-based protein precipitation method, the two-phase liquid extraction method significantly increased the metabolite coverage by 20.29%. Besides, the proposed pseudotargeted metabolomics method exhibited higher sensitivity and better repeatability than the untargeted method. Finally, we applied the established pseudotargeted method to the metabolomics study of depressive rats and screened 53 differential variables. Sixteen determined differential metabolites were mainly in four metabolic pathways including glycerophospholipid, arachidonic acid, sphingolipid metabolisms, pentose and glucuronate interconversions. The results indicated that the pseudotargeted method based on two-phase liquid extraction broadened the metabolite coverage with good sensitivity and repeatability, exhibiting significant potential for discovering differential metabolites in metabolomics studies.
研究领域:
分析化学
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代谢组学
·
医学
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PubMed
高影响因子
EUROPEAN FOOD RESEARCH AND TECHNOLOGY
·
2023
·Vol. 249
·期 8
·2017-2027
·
IF 3.3
Han Zai-Gang,Zhang Lingli,Qi Chao,Shi Qing,Min Jun Zhe
The detection and analysis of α-dicarbonyl compounds (α-DCs) in food can guide the daily diet of patients with various chronic diseases. However, these compounds have poor stability, lack color-generating groups, and have low ionization efficiency. Therefore, it is difficult to monitor them. We established a new simple and sensitive method for the simultaneous determination of four α-DCs, including glyoxal (GO), methylglyoxal (MG), 2,3-butanedione (DMGO), and 3-deoxyglucosone (3-DG) in beer by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) with pre-column derivatization using 3-benzyl-2-oxo-4λ 3 -thiazolidine-4-carbohydrazide (BOTC), a novel MS probe for targeted identification of carbonyl compounds. α-DCs were derivatized with BOTC at 60 °C for 60 min, and the gradient analysis was carried out on a CSH C18 (2.1 mm × 50 mm; 1.7 μm) column for 5 min with a mobile phase A of 0.1% formic acid (FA) in water and mobile phase B of 0.1% FA in acetonitrile. The linearity range of this method was 0.39–500 μM ( R 2 ≥ 0.9995). The limits of detection (LOD) were in the range of 13–50 fmol. The average recoveries of α-DCs were 95.15–101.67%. This method was successfully applied to the detection of α-DCs in beer; the content of 3-DG was the highest, several hundred times higher than that of GO, MG, and DMGO, and the difference was significant. This new BOTC derivatization-based UHPLC-MS/MS method for the simultaneous detection of four α-DCs in beer is highly sensitive and can be used for the detection of α-DCs in alcoholic beverages. Graphical abstract
研究领域:
食品科学
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分析化学
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高影响因子
JOURNAL OF FOOD SCIENCE AND TECHNOLOGY-MYSORE
·
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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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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高影响因子
Oil Crop Science
·
2026
·
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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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
·
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
·
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
·
生物技术
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
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 CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
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
·
分析化学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）