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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2019 · IF 2.983

Permeability and transport mechanism of trihexyphenidyl hydrochloride in Caco-2 cell monolayer model with a validated UPLC-MS/MS method

Chengcan Lu,Kejia Fu,Kangna Cao,Jiali Wei,Jing Zhou,Di Zhao,Ning Li,Yang Lu,Xijing Chen,Yongjie Zhang

A rapid and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was applied to investigate the permeability characteristics and transport mechanism of trihexyphenidyl hydrochloride (TH) in D-hanks with the Caco-2 cells model. Analytes were separated using an Zorbax Extend-Agilent C 18 (1.8 μm, 4.6 × 30 mm) column following a simple methanol precipitation treatment. The mobile phase consisted of methanol and water containing 0.1% formic acid, and the total gradient program time was 1.5 min. Method validation results showed TH was linear in 2–500 ng/mL (r 2  > 0.99), and the lower limit of quantification (LLOQ) was 2 μg/mL. The intra-run and inter-run precision (coefficient of variation, CV) was within 2.80%, and the accuracy (relative error, RE) was within ±11.10%. Stability of TH was evaluated in different storage conditions, including short-term I-III, long-term I-III, 2 and 4 h in the artificial gastrointestinal tract, respectively. There was no obvious interference between TH and internal standards (IS). With the established Caco-2 monolayer permeability model, Papp(AB) of TH was calculated as 46.29 ± 8.31 × 10 −6  cm/s, and the efflux ratio (ER) value was calculated as 0.22, indicating a high permeability character of TH. The transmembrane transport of TH followed the concentration-dependent, temperature-independent, and energy-free manner. Collectively, these characteristics indicate that TH is a highly permeable drug and the transport mechanism is mainly via passive diffusion.

CAS / MDL: 15676-16-1
研究领域: 药理学 · 药物代谢动力学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH · 2021 ·Vol. 29 ·期 15 ·21826-21838 · IF 4.223

Simultaneous detection of ten kinds of insecticide residues in honey and pollen using UPLC-MS/MS with graphene and carbon nanotubes as adsorption and purification materials

Pang Xiuyu,Li Chenyu,Zang Chuanjiang,Guan Lei,Zhang Peng,Di Chunxiang,Zou Nan,Li Beixing,Mu Wei,Lin Jin

An analytical method of simultaneous detection of ten insecticide residues in honey and pollen was established. The samples were purified with QuEChERS approach using new adsorbents and analyzed with UPLC-MS/MS. The results showed that both of graphene and carbon nanotubes were highly efficient adsorbents for the dSPE clean up to eliminate coextractives in the samples, and graphene was superior to carbon nanotubes for the detection of pesticide residues in honey and pollen samples. The proposed method was used to detect pesticide residues in 25 honey samples and 30 pollen samples which were randomly collected from more than ten provinces in China. All honey samples contain 1–27 μg/kg of chlorpyrifos residues. Only 4% of the honey samples were detected containing acetamiprid and imidacloprid, while the other seven pesticides were not detected. Chlorpyrifos residues were found in all pollen samples (5–66 μg/kg), among which twenty percent exceeded the maximum residue limits (MRLs, 50 μg/kg, European Commission Regulation). Most of the pollen samples containing pesticide concentrations higher than MRLs were collected from rape, followed by lotus, camellia, and rose. Besides, 36.7% and 33.3% of the pollen samples had imidacloprid and flupyradifurone higher than 5 μg/kg. A total of 26.7% pollen samples were detected containing bifenthrin, while none of the other six pesticides were detected in pollen samples.

研究领域: 分析化学 · 食品科学 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2025 · IF 2.8

High-throughput screening of 311 new psychoactive substances and metabolites in wastewater by direct injection UPLC-MS/MS

Yue Xiao,Shuai Yuan,Ruxin Luo,Ruiqin Zhu,Qiongying Zheng,Bin Di,Ping Xiang

The rapid global spread of new psychoactive substances (NPS) in recent years has become an issue in many countries. One emerging technology that can provide early warnings and assessments of drug situations is the monitoring of NPS in wastewater. In this study, we developed and optimized a high-throughput qualitative screening method based on direct injection that enabled the simultaneous detection of 311 NPS and metabolites (87 synthetic cannabinoids, 43 synthetic cathinones, 71 phenylethylamines, 10 tryptamines, 40 phencyclidines, 9 benzodiazepines, 38 fentanyls, and 13 piperazines) in municipal wastewater. The run time for drug detection was only 16 min, and the method was validated to perform well in terms of selectivity, limit of detection (LOD), recovery, and matrix effect. Overall, 95.8 % of the targets had an LOD ≤10 ng/L and the recoveries ranged from 71.01 % to 119.88 %. The method was validated on 976 real samples from a city in China, and 32 substances were detected, with the highest detection rate for ketamine. This study provides a simple and direct analytical method for wastewater monitoring, which will aid in combating drug-related crime and maintaining social stability as new NPS continue to enter global markets.

CAS / MDL: 1336-21-6
研究领域: 环境科学 · 毒理学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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International Journal of Analytical Chemistry · 2020 · IF 1.678

An UPLC-MS/MS Method for Determination of Osimertinib in Rat Plasma: Application to Investigating the Effect of Ginsenoside Rg3 on the Pharmacokinetics of Osimertinib

Zhenzhen Ying,Jingyao Wei,Ruijuan Liu,Fang Zhao,Yifang Yu,Xin Tian

Osimertinib is a novel oral, potent, and irreversible epidermal growth factor receptor tyrosine kinase inhibitor (EGFR-TKI) for treatment of advanced T790M mutation-positive advanced non-small cell lung cancer, which is commonly combined with ginsenoside Rg3 in clinic to enhance the efficacy and minimize adverse reactions. In the present study, a highly sensitive UPLC-MS/MS method was established and validated for analysis of osimertinib in rat plasma according to US FDA guideline. Separation was performed on a C18 (2.1 × 50 mm, 2.6 μm) column using a gradient elution of ammonium formate (10 mM) with 0.1% formic acid buffer (A) and ACN (B) at a flow rate of 0.2 mL/min. Detection was carried out on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization in the MRM mode. The method was validated over a concentration range of 1–400 ng/mL for osimertinib. The intra- and interday accuracy and precision values were within ±15%. No significant degradation occurred under the experimental conditions in stability assays. There was a further investigation on the effects of multiple doses of ginsenoside Rg3 on the pharmacokinetics of osimertinib in rats for the first time. The results implied that osimertinib exhibited a slow absorption and moderate-rate elimination in rats following oral administration. Coadministeration with ginsenoside Rg3 (5 mg/kg, 7 days, i.g.) may have no effect on the pharmacokinetics of osimertinib in rats. The results provide a reference for the clinical concomitant medications of Rg3 and osimertinib.

研究领域: 药物分析 · 肿瘤学 · 药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CONTROL · 2022 · IF 6.652

Structural annotation and discovery of toxic cyclopeptides and their analogues in lethal mushroom Amanita and Lepiota species using UPLC-HRMS and molecular networking strategy

Zhiyong Zhao,Hengchao E,Enjing Tian,Tingting Fan,Xianli Yang,Xiaobei Li,Yanmei Zhang,Xujiao Li,Ailiang Chen,Changyan Zhou,Xiaoyan Zhao

Foodborne poisoning caused by the cyclopeptide toxins-producing mushroom species seriously endangers human life health. In recent years discovery of new cyclopeptides is getting more attention not only for their toxicity but also for their specific bioactivity. In this study, a combined strategy using liquid chromatography tandem high resolution mass spectrometry and the feature-based molecular networking analysis was established to identify the known cyclopeptide toxins and discover new cyclopeptides in the cyclopeptide toxins-producing mushroom species. The specific fragmentation behaviors of the known cyclopeptide toxins were systematically annotated. Four new phallotoxin analogues were identified for the first time, the chemical structures of which were completely deduced. Moreover, the chemical profiles of the toxic cyclopeptides in lethal mushroom Amanita and Lepiota species were investigated by the self-built cyclopeptides database. The developed strategy could be utilized as a useful tool for identifying the cyclopeptide toxins-induced food poisoning , as well as aid in the discovery of more unknown cyclopeptides.

CAS / MDL: 540-69-2 7647-01-0
研究领域: 食品科学 · 毒理学 · 分析化学
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Food Bioscience · 2024 · IF 4.8

Application of silanized melamine sponges in matrix purification for rapid analysis of multiple pesticides and veterinary drugs in honey by UPLC-MS/MS

Baocheng Ji,Lanrui Yang,Mengxian Zhang,Peiyu Li,Zhuchen Hou,Jia Lv,Xu Xu,Wenbao Bi,Gaigai Xu,Yanhong Bai

In this study, a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method based on two kinds of silanized melamine sponges coupled with ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) were developed for the determination of multiple pesticides and veterinary drugs in honey. Quick and convenient matrix separation could be achieved with the developed silanized melamine sponges by simply soaking and squeezing. At three spiked levels, all recoveries of the monitored drugs ranged from 63.6% to 114.8%, with relative standard deviations less than 17.7%. No significant matrix influence was observed with matrix effects within −13.9%∼+15.1% for all monitored drugs. Good linearity with correlation coefficient (R 2 ) ≥0.991 was obtained in the range of 0.08–100 μg kg −1 for most drugs. The limits of detection and quantification ranged from 0.04 to 3.6 μg⋅kg −1 and from 0.08 to 9.8 μg⋅kg −1 , respectively. The results had shown the satisfactory matrix purification performance of silanized melamine sponges and indicated its good application prospect in the multiple determination of pesticides and veterinary drugs in various foods.

研究领域: 食品科学 · 分析化学
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CyTA-Journal of Food · 2022 · IF 2.478

Profiling of volatile and non-volatile compounds in Dianhong by a combined approach of static headspace GC-MS and UPLC-MS

Yanzhi Sun,Yingjie Fu,Rirong Chen,Yipeng Zhang,Tougen Liao,Hui Xi,Shihao Sun,Zhihong Cheng

The systematic identification of volatile organic compounds (VOCs) and non-VOCs will facilitate understanding the characteristic aroma and bioactive constituents of Dianhong. This article reported for the first time the volatile and non-volatile composition profiles of Dianhong from four main producing areas. A combined total of 42 VOCs were identified from four Dianhong samples by static headspace GC-MS. Thirteen VOCs were found to be important common components contributing to the characteristic aroma of Dianhong. The non-VOCs of Dianhong were evaluated by UPLC-ESI-MS, and Dianhong samples from four producing areas shared almost the same component profiles. Thirty-four components including derivatives of quinic acid, gallic acid, and catechin, flavone C-glycosides, flavonol O-glycosides, and alkaloids were characterized. Finally, catechin, gallic acid, 5-O-galloylquininc acid, and theobromine were characterized as the main non-VOCs in Dianhong. Dianhong samples from four main producing areas showed similar VOCs and non-VOCs profiles under our optimized GC-MS and LC-MS conditions.

研究领域: 食品科学 · 分析化学 · 植物学
✓ 已验证 DOI 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Preparation of thiol-free amino acid plasma matrix for quantification of thiol amino acids and their oxidized forms in human plasma by UPLC-MS/MS

Ting Tao,Yuyu Cao,Liping Zhang,Dayi Xu,Kaiyuan Pang,Yanli Li,Xiaobao Wei,Zengxian Sun

Thiol amino acids, with great physiological significance, are unstable, and have small molecular weights, as well as very low endogenous concentrations. Therefore, to quantitatively and directly analyze them using liquid chromatography-tandem mass spectrometry is difficult. To overcome these problems, we aimed to prepare a thiol-free amino acid plasm matrix as blank sample to reduce the background for the first time. Using compounds with maleimide group that react with classical thiols to generate water-insoluble products. Reducing agents Tris(2-carboxyethyl)phosphine (TCEP) was applied to cooperate with bismaleimide (DM) for elimination of thiol amino acids from plasma 10 min at room temperature and pH 7. Further, the residual TCEP from plasma were removed using an anion exchange resin within 10 min. Methodological validation analysis revealed good performance in linearity, precision, extraction recovery (≥ 82 %), and stability (except oxidized glutathione). This quantitative analysis was successfully applied to blood samples of 9 people in good health. This study provides a foundation for the development of accurate and rigorous quantitative analysis methods targeting thiol amino acids in different body fluids or tissues. Moreover, it paves the way toward realizing several clinical applications.

研究领域: 生物化学 · 临床医学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2023 ·Vol. 28 ·期 4 ·1947 · IF 4.6

Investigation on Antioxidant Activity and Different Metabolites of Mulberry (Morus spp.) Leaves Depending on the Harvest Months by UPLC–Q-TOF-MS with Multivariate Tools

Zili Guo,Jiangxuan Lai,Yiwen Wu,Sheng Fang,Xianrui Liang

The changes in active components in mulberry leaves harvested in different months and their antioxidant activities were investigated. Ultra-high-performance liquid chromatography–tandem quadrupole time-of-flight mass spectrometry (UPLC–Q-TOF-MS) with multivariate statistical tools was used to investigate the chemical constituents in the extracts of mulberry leaves. The results indicated that mulberry leaves were rich in phenolic acids, flavonoids, organic acids, and fatty acid derivatives. In addition, 25 different compounds were identified in the different batches of mulberry leaves. The 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity was measured to evaluate the in vitro antioxidant activities of mulberry leaves. Among the four batches, batch A, harvested in December, exhibited the strongest DPPH radical-scavenging activity, while batch B, harvested in March, showed the weakest activity. This was related to the total phenolic content in the mulberry leaves of each batch. The optimal harvest time of mulberry leaves greatly influences the bioactivity and bioavailability of the plant.Keywords:mulberry leaf;chemical constituent;antioxidant;UPLC–Q-TOF-MS;free radical scavenging activity

CAS / MDL: 64-18-6
研究领域: 生药学 · 分析化学 · 植物科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Frontiers in Pharmacology · 2025 · IF 4.8

UPLC-MS/MS method for simultaneous determination of pyrantel, praziquantel, febantel, fenbendazole and oxfendazole in dog plasma and its application to a bioequivalence study

Fengyichi Zhang,Fanxi Guo,Xinyu Zhao,Chongyang Li,Junli Wang,Mengyun Wang,Ruixia Ma,Baochang Chen,Qiangqiang Miao,Yimeng Wang,Zihan Wang,Di Cao,Zugong Yu

A rapid, sensitive and reliable ultra–performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the simultaneous quantitation of pyrantel (PYR), praziquantel (PRA), febantel (FBT) and its active metabolites, fenbendazole (FEN) and oxfendazole (OXF) in dog plasma. Fenbendazole–D3 (FEN–D3) was used as an internal standard (IS). The analytes and IS were prepared using simple protein precipitation (PP) combined with liquid–liquid extraction (LLE). Chromatographic analysis was performed on UPLC BEH C18 column using acetonitrile–0.1% formic acid in water for gradient elution. Detection was carried out in multiple reaction monitoring (MRM) mode under positive electrospray ionization. The standard curves were linear through the concentration range of 4–240 ng/mL for PYR and OXF, 15–900 ng/mL for PRA, 2–120 ng/mL for FBT and 10–600 ng/mL for FEN with all correlation coefficients >0.99. The intra–and inter–batch precision was 1.08%–14.26% and accuracy was from 90.66% to 110.28%. The mean extraction recoveries for the analytes and IS were >90%. The total run time was 9.0 min. The developed method was successfully applied to a bioequivalence study after oral administration of compound febantel tablets in 38 healthy dogs.

CAS / MDL: 1336-21-6
研究领域: 兽医学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD RESEARCH INTERNATIONAL · 2024 · IF 7

Untargeted metabolomics analysis using UPLC-QTOF/MS and GC–MS to unravel changes in antioxidant activity and compounds of almonds before and after roasting

Xiao Shan,Lin Li,Yu Liu,Ziwei Wang,Binbin Wei,Zhongbo Zhang

Almonds are a commonly consumed nut. They possess significantof nutritional and health benefitsand are commonly processed by roasting. This study aimed to investigatthe effects of roasting on the compound composition and antioxidant activity of almonds. Metabolomics analysis, performed via UPLC-QTOF/MS, and fatty acid analysis, conducted via GC–MS, employed, and the results demonstrated a significant increase in antioxidant activity of post-roasting and in vitro digestion, ranging from 1.16 to 3.44 times. Untargeted metabolomics identified a total of 172 compounds, with notable differences observed in organic oxides, fatty acids, and their derivatives. Correlation analysis identified fatty acids as the primary influencers of changes in antioxidant activity following roasting. Taken together, these findings suggest that roasting enhances the antioxidant activity of almonds, primarily due to alterations in fatty acid analogs, thereby providing valuable insights into optimizing almond consumption for health benefits.

研究领域: 食品科学 · 营养学 · 分析化学 · 代谢组学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2023 ·Vol. 12 ·期 16 ·3000 · IF 5.2

Investigation of the Potential Phlorotannins and Mechanism of Six Brown Algae in Treating Type II Diabetes Mellitus Based on Biological Activity, UPLC-QE-MS/MS, and Network Pharmacology

Jialiang Chen,Zheng Zhou,Ping Li,Shuhong Ye,Wei Li,Ming Li,Lin Zhu,Yan Ding

Type 2 diabetes mellitus (T2DM) has developed into an important health concern worldwide. The discovery of phlorotannins and their efficacy in the treatment of T2DM has become a hotspot for research in various fields. In this study, the potential phlorotannins and mechanism of six brown algae against T2DM were in-depth investigated using biological activity assays, LC-MS, and network pharmacology. First, the ethyl acetate fraction (EA frac.) showed high polyphenolic content and possessed significantly antioxidant and enzyme inhibitory abilities. Further, a total of fifty-nine peaks were obtained from six EA fracs. via UPLC-QE-MS/MS analysis, and fifteen of them were identified as phlorotannins and their isomers or derivatives. In detail, the chemical structures of six phlorotannins were inferred as dibenzodioxine-1,3,6,8-tetraol, bifuhalol, dioxinodehydroeckol, eckol, fucofurodiphlorethol, and fucotriphlorethol; three phlorotannin isomers were deduced to be fucophlorethol, trifucol, triphlorethol A, or triphlorethol B; and the phlorotannin derivative ofm/z263 was determined to be dibenzodioxine-1,2,3,6,8-pentanol or dibenzodioxine-1,2,4,5,7-pentanol. Moreover, 43 T2DM-related targets acted on by these chemicals were identified, and the function of phlorotannin to prevent and treat T2DM was elucidated in a holistic way based on the established compound-target-disease network, and GO function and KEGG pathway enrichment analysis.Keywords:phlorotannins;T2DM;UPLC-QE-MS/MS;network pharmacology

研究领域: 药理学 · 生物化学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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