Foods
·
2025
·Vol. 14
·期 14
·2421
·
IF 5.1
Mengqiong Yang,Guangming Mei,Daoxiang Huang,Xiaojun Zhang,Pengfei He,Si Chen
A sensitive method was developed for detecting diazepam residues in aquatic products using magnetic dispersive solid-phase extraction (MDSPE) coupled with ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). Samples extracted with 1% ammonia–acetonitrile were purified using synthesized Fe3O4@SiO2-PSA nanoparticles via MDSPE before UPLC-MS/MS analysis. Separation was performed on a C18column with gradient elution using 0.1% formic acid–2 mM ammonium acetate/methanol. Detection employed positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. Characterization confirmed Fe3O4@SiO2-PSA’s mesoporous structure with excellent adsorption capacity and magnetic properties. The method showed good linearity (0.1–10 μg/L,r> 0.99) with an LOD and LOQ of 0.20 μg/kg and 0.50 μg/kg, respectively. Recoveries at 0.5–15.0 µg/kg spiking levels were 74.9–109% (RSDs 1.24–11.6%). This approach provides rapid, accurate, and high-precision analysis of diazepam in aquatic products, meeting regulatory requirements.
研究领域:
分析化学
·
食品安全
·
材料科学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Tong Wu,Libin Pu,Wenqing Liu,Yinliang Bai,Jingjing Ma,Xia Song,Aijia Cao,Shunli Pan,Jiahui Yang,Chang Wang,Wen Qiu
Objective To develop a rapid, convenient, accurate, and low-residual-effect ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method for the determination of polymyxin B sulfate and colistin sulfate in the blood of patients with multidrug-resistant bacterial infections, as well as caspofungin acetate in the blood of patients with fungal infections, thus facilitating the rational use of antibiotics in clinical applications. Methods All analytes were diluted with 0.2 % aqueous formic acid, and plasma proteins were precipitated using acetonitrile. The selected reaction monitoring (SRM) mode was used for measurement. Separation of all analytes was completed on a Hypersil GOLD C18 column (100 × 2.1 mm, 3.0 µm). They were quantitatively analyzed using electrospray ionization on a triple quadrupole mass spectrometer in the positive ion mode. The mobile phase consisted of water (containing 0.1 % formic acid) and acetonitrile, which was delivered by gradient elution at a flow rate of 0.3 ml/min. The internal standard was bacitracin zinc (BcZn), and the column temperature was maintained at 25 °C. The runtime for each analysis was 3.5 min. Results The procedure was validated following the recommendations of the U.S. Food and Drug Administration, which included measurements of accuracy (ranging from 83.27 % to 105.86 % for within-run and between-run accuracy), precision (with coefficients of variation from 2.50 % to 16.51 % for within-run precision and between-run precision), and matrix effects (ranging from 88.65 % to 103.94 %). The extraction recoveries ranged from 38.01 % to 42.76 for polymyxin B1 (PMB1), polymyxin B2 (PMB2), polymyxin E1 (PME1), polymyxin E2 (PME2), and 88.65 % to 89.84 % for caspofungin (CPF). Plasma samples were stable under various storage conditions, including three freeze–thaw cycles at −80 °C, 24-hour periods at room temperature and 4 °C, and 30 days of freezing at both −20 °C and −80 °C, with relative standard deviations (RSD) of less than 15 %. Conclusion In this study, a UPLC–MS/MS method was developed to simultaneously quantify PMB1, PMB2, PME1, PME2, and CPF in human plasma. The method was validated in blood samples from patients with multidrug-resistant bacteria combined with fungal infections and is suitable for therapeutic drug monitoring.
研究领域:
临床药理学
·
分析化学
·
感染病学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Mingyu Pan,Wenfeng Geng,Yuanxiao Wang,Makoto Tsunoda,Jiatong Liu,Yingxia Zhang,Haimei Yang,Lu-shuang Li,Shiwen Song,Jinqiang Liang,Yanting Song
Areca nuts have been used as a traditional Chinese medicine (TCM) for thousands of years. Recent studies have shown that it exhibits good pharmacological activity and toxicity. In this study, the pharmacokinetics of five major components of areca nut extract in rats were investigated using a highly sensitive ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) method. Arecoline, arecaidine, guvacoline, guvacine, and catechin were separated and quantified accurately using gradient elution with mobile phases of (A) water containing 0.1 % formic acid-10 mM ammonium formate, and (B) methanol. The constituents were detected under a timing switch between the positive and negative ion modes using multiple reaction monitoring (MRM). Each calibration curve had a high R 2 value of >0.99. The method accuracies ranged −7.09–11.05 % and precision values were less than 14.36 %. The recovery, matrix effect, selectivity, stability, and carry-over of the method were in accordance with the relevant requirements. It was successfully applied for the investigation of the pharmacokinetics of these five constituents after oral administration of areca nut extract. Pharmacokinetic results indirectly indicated a metabolic relationship between the four areca nut alkaloids in rats. For further clarification of its pharmacodynamic basis, this study provided a theoretical reference.
研究领域:
药理学
·
分析化学
·
中药学
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DOI
PubMed
高影响因子
Food Analytical Methods
·
2018
·Vol. 11
·期 6
·1780-1788
·
IF 2.245
Zhao Zhiyong,Yang Xianli,Zhao Xiaoyan,Chen Lei,Bai Bing,Zhou Changyan,Wang Jianhua
Fusarium species are one of the common pathogenic fungi of vegetable diseases. Some Fusarium species produce toxic secondary metabolites, which have potential health risks for humans and animals. In the study, an ultra-performance liquid chromatography tandem mass spectrometry method (UPLC-MS/MS) was developed for the analysis of 13 emerging and traditional Fusarium toxins in pepper, tomato, cucumber, and potato. Samples were extracted by a modified quick, easy, cheap, effective, rugged, and safe method. Dispersive solid-phase extraction was employed for the removal of matrix interferences from the crude extracts of various vegetables. Matrix effect was compensated using matrix-matched calibration curves. The method was fully validated according to the European Commission Decision 2002/657/EC. For all the targeted analytes, good linearity ( R 2 ≥ 0.9823) was obtained. Recoveries were in the range of 62 and 114% in pepper, tomato, cucumber, and potato, with intra-day relative standard deviations lower than 14.3%. Quantitation limits of the developed method were between 0.25 and 20 μg/kg in four sample matrices. The method was successfully employed for the analysis of Fusarium toxins in vegetable samples.
研究领域:
食品科学
·
毒理学
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DOI
高影响因子
Thoracic Cancer
·
2023
·Vol. 14
·期 33
·3331-3341
·
IF 2.9
Mengming Xia,Xueyi Song,Zebei Lu,Yu Wang,Quan Zhou,Peiwu Geng,Shuanghu Wang,Yunfang Zhou,Qingjun Wu,Aixia Han
Background Lenvatinib is a multitargeted tyrosine kinase inhibitor used in the treatment of a variety of solid tumors. This study aims to investigate the potential pharmacokinetic interactions between lenvatinib and various azoles (ketoconazole, voriconazole, isavuconazole and posaconazole) when orally administered to rats. Methods A total of 30 Sprague–Dawley rats were randomly allocated into five groups and administered 20 mg/kg of ketoconazole, voriconazole, isavuconazole and 30 mg/kg of posaconazole and 0.5% CMC-Na, through gavage for a duration of 7 days prior to the commencement of the experiment. On the final day, the rats were given 10 mg/kg of lenvatinib. The blood concentration of lenvatinib was determined using UPLC-MS–MS. In vitro lenvatinib were incubated with azoles and rat liver microsomes (RLMs) or human liver microsomes (HLMs). Molecular docking was lastly used to examine the binding strength of the enzymes and ligands with Autodock Vina. Results AUC and C max of lenvatinib significantly increased with each of the azoles ( p < 0.05), whereas CLz/F decreased 0.83-flod, 0.41-fold ( p < 0.05) and 0.72-fold ( p < 0.01) in voriconazole, isavuconazole and ketoconazole in rats. The IC50 of lenvatinib with the azoles were 0.237, 1.300, 0.355 and 2.403 μM in RLMs and 0.160, 1.933, 3.622 and 1.831 μM in HLMs. Molecular docking analysis suggested that azoles exhibited a strong binding ability towards the target enzymes. Conclusion It is imperative to acknowledge the potential drug–drug interactions mediated by CYP3A4 between azoles and lenvatinib, as these interactions hold significant implications for their clinical utilization.
研究领域:
药理学
·
临床医学
·
分子生物学
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产品关联
DOI
PubMed
高影响因子
FOOD CONTROL
·
2022
·
IF 6.652
Gaozhen Li,Fukai Guan,Shancang Zhao,Huihui Xu,Jiashuai Sun,Jingcheng Huang,Qingqing Yang,Yanyin Guo,Xia Sun,Yemin Guo
As an organochlorine pesticide, procymidone has become an increasing serious problem in vegetables in recent years. In order to solve a series of problems such as low sensitivity of the immunological methods, a time-resolved fluorescent immunoassay strip (TRFIAS) was developed with low limit of detection (LOD). Based on the principle of antigen-antibody immune competition, TRFIAS could detect procymidone in vegetables. After the targets being added, the samples were incubated at 37°C for 10 min. TRFIAS was observed under a UV lamp of 365 nm. The results were processed by ImageJ software to complete the qualitative and quantitative analysis of TRFIAS. Under the optimal working conditions, a linear range of TRFIAS was 5–250 ng/mL with a LOD of 0.33 ng/mL and a visual limit of detection (VDL) of 50 ng/mL. And the TRFIAS had good specificity, precision and accuracy. Comparing the results of TRFIAS with those of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), the two assays were in good agreement. Therefore, TRFIAS has the advantages of high sensitivity, high specificity, simple operation and relatively short assay time. Meanwhile, it shows absolutely great advantages in both quantitative and qualitative analysis.
研究领域:
农业化学
·
分析化学
·
食品科学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Jieyu Zhang,Yan Chen,Wenxiang Fan,Linnan Li,Yueming Ma,Zhengtao Wang,Rong Shi,Li Yang
The combined efficacy in lowering serum lipid levels and increasing kidney protection of Plantago asiatica L. seed (Plantago) and Coptis chinensis Franch. rhizoma (Coptis) is far better than the effects of either herb alone. This finding suggests that there must be some degree of herb-herb interactions (HHI) affect potency. Here, we chose geniposidic acid (GPA), acteoside (ACT), and plantagoamidinic acid A (PLA) as active components in Plantago, and berberine (BBR) as the active component in Coptis, and, using transporter gene-transfected Madin-Darby canine kidney (MDCK) cells in combination with specific substrates and inhibitors, investigated Plantago- Coptis HHIs. We also established a UPLC-MS/MS analytical method to determine substrate content. Results showed that PLA in Plantago was a substrate of rOCT1/2 and rMATE1, and had inhibitory effects on rOCT2 and rMATE1. We also found that ACT is a substrate of rMATE1, but GPA was not a substrate of any transporter that we investigated. When BBR was used as the substrate, the inhibition rate of 10 μM PLA was 53.6% on rOCT2 and 31.5% on rMATE1. The inhibition rates of 30 μM ACT and 30 μM GPA on rMATE1 were 47.0% and 31.0%, respectively. Thus, our findings suggest that GPA, ACT, PLA, and BBR have competitive interactions that are driven by the rOCT2 and rMATE1 transporters. These interactions affect the transport and excretion of compounds and result in efficacy changes after co-administration.
研究领域:
药理学
·
药学
·
中药学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2022
·
IF 16.744
Zhe Zhao,Wuming Xie,Zijun Huang,Haiming Cai,Yuemeng Ji,Baocong Zhao
The antibiotic florfenicol (FF) discharged into the aquatic environment may cause serious water pollution. Therefore, an effective way to eliminate FF antibiotics from the water bodies should be proposed. Herein, MIL-53(Al)-supported nano zero-valent iron (NZVI@MIL-53(Al)) was synthesized and applied to activate hydrogen peroxide (H 2 O 2 ) to spark the Fenton reaction for FF antibiotics removal. The characterization results demonstrated the successful loading and good dispersion of NZVI onto MIL-53(Al). 100 % FF antibiotics degradation could be achieved under the optimal reaction conditions, including an initial FF antibiotics concentration of 20 mg L −1 , initial solution pH of 3.0, NZVI@MIL-53(Al) dose of 25 mg L −1 , and H 2 O 2 concentration of 0.2 mM. And after four cycles, the FF antibiotic degradation efficiency was still 81.18 %. The lowest tolerance for HCO 3 − was observed while the degradation activity was maintained at the presence of Cl − and HA. EPR measurement and free radical quenching experiment showed that ·OH was the main reactive specie in the NZVI@MIL-53(Al)/H 2 O 2 system. FF antibiotics degradation involved hydroxylation reactions (electrophilic substitution), dehalogenation, hydrolysis, and cleavage based on the UPLC-MS/MS analysis and DFT calculation. Noteworthy, 0.247 mg L −1 of F − and 1.2 mg L −1 of Cl − were detected in the solution after the reaction due to the breakage of the stable C–Cl bond and C–F bond. Finally, this work revealed that the NZVI@MIL-53(Al), with high stability and recyclability, could be a potential heterogeneous catalyst for treating antibiotic wastewater.
研究领域:
环境科学
·
化学工程
·
材料科学
·
分析化学
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产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
You Long,Yuting Wang,Gan Zhang,Bei Gan,Qiang Yu,Jianhua Xie,Xinyi Zang,Yi Chen
Enniatin and Alternaria mycotoxins have presented adverse effects to food safety and human health, and an accurate, simultaneous analytical method for these mycotoxins was promising. This study reported the synthesis of a magnetic covalent organic framework (NH 2 -Fe 3 O 4 @TpBD-COF) for efficient extraction of seven mycotoxins from wheat, coupled to UPLC-MS/MS for simultaneous quantification. The magnetic solid phase extraction (MSPE) parameters, including adsorbent dose (10 mg), vortex duration (5 min), and extraction/elution solvents (ACN/MeOH, 6/4, v /v), were systematically optimized. Method validation revealed ultra-low limits of quantification (LOQs:0.03 to 0.5 μg kg −1 ), matrix effects (ME<8.49 %), recovery rates(81.3 %–109 %), and precision (RSD < 9.70). The adsorbent maintained satisfactory performance through 8 reuse cycles. Density functional theory (DFT) calculation indicated exergonic adsorption, primarily driven by hydrogen bonding, van der Waals forces, and hydrophobic interactions. The integrated method offers a sensitive and accurate approach for emerging mycotoxin analysis in wheat, potentially mitigating associated health risks.
研究领域:
食品安全
·
分析化学
·
真菌毒素学
·
材料科学
·
环境卫生
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CURRENT DRUG METABOLISM
·
2021
·Vol. 22
·期 1
·70-82
·
IF 3.731
Zuo Lihua,Li Jia,Xue Lianping,Jia Qingquan,Li Zhuolun,Zhang Mengya,Zhao Mengfan,Wang Mengli,Kang Jian,Du Shuzhang,Sun Zhi
Background: Alpiniae oxyphyllae Fructus (AOF), a traditional Chinese medicine (TCM), is widely used in the treatment of urinary, gastrointestinal and neurologic diseases in China. Although terpenoids are the main active ingredients of AOF, there are few researches on their pharmacokinetics
and metabolism. Methods: In this study, a sensitive, rapid, accurate and novel ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established to evaluate the pharmacokinetic behavior of five terpenoids (oxyphyllenodiol B, (4S* ,5E,10R*)-7-oxo-tri-nor-eudesm-5-en-4β-ol,
7-epi-teucrenone, (+)- (4R,5S,7R)-13-hydroxynootkatone, (E)-labda-12,14-dien-15(16)-olide-17-oic acid) in rats after oral administration of AOF extracts. 27 metabolic metabolites of the five terpenoids were identified by ultra high performance liquid chromatography -Q Exactive hybrid quadrupole-orbitrap
high-resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS) based on precise mass and fragment ions. Results: The established pharmacokinetic analysis method showed good linearity over a wide concentration range, and the lower quantitative limit (LLOQ) ranged from 0.97 to 4.25
ng/mL. Other validation parameters were within the acceptable range. In addition, 27 metabolites were identified in plasma, urine and feces samples, and the metabolic pathways of five terpenoids were mainly focused on glucoside conjugation, dehydration, desaturation and glycine conjugation.
Conclusion: This is the first study on the pharmacokinetics and metabolism of five terpenoids in AOF, illuminating the disposal process of terpenoids in vivo. It was expected that the results of this study would provide some references for the apprehension of the action mechanism and
the further pharmacological study of five terpenoids in AOF.
研究领域:
中药学
·
分析化学
·
药理学
✓ 已验证
DOI
高影响因子
RSC Advances
·
2026
·Vol. 16
·期 31
·28230-28242
·
IF 6.1
Jin-tuo Yin,De-mao Wang,Xue-chun Wu,Juan Lu,Zheng-ming Qian,De-qiang Li,Rui Feng
Taihangia rupestris Yu & Li (T. rupestris) was a nationally protected plant and its active compounds exhibit antidiabetic potential, but systematic phytochemical and pharmacological investigations remain limited. To balance conservation and utilization, the chemical composition and bioactivities (antioxidant and α-glucosidase inhibitory effects) of wild and cultivated T. rupestris were compared, followed by active compound screening. UPLC-MS/MS was used to identify chemical constituents in wild, mountain-cultivated, and foothill-cultivated samples, with multivariate analysis for differential components. The TFC and TPC, and the antioxidant capacity were evaluated via FRAP, CUPRAC, TRC, and DPPH assays. Additionally, α-glucosidase inhibition was assessed via IC50 determination. Online HPLC-ABTS and ultrafiltration-LC/MS (UF-LC/MS) were employed to screen antioxidants and α-glucosidase inhibitors (α-GIs), respectively, with molecular docking validating binding mechanisms. As a result, among 114 identified compounds, 111 showed significant environment-dependent variations, primarily flavonoids, phenolics, and terpenoids. Foothill-cultivated plants exhibited upregulated flavonoids/phenolics (e.g., rutin and gallic acid derivatives, P < 0.05) and superior antioxidant activity (Trolox equivalents: FRAP 367.18 ± 1.03; CUPRAC 572.40 ± 0.82) and α-glucosidase inhibition (IC50 0.2775 µg mL−1) versus wild (IC50 0.4948 µg mL−1) and mountain-cultivated samples (IC50 0.5425 µg mL−1). Ten antioxidants were screened, with seven also acting as α-GIs. UF-LC/MS and docking confirmed 8 α-GIs (binding energy < −5 kcal mol−1), where phenolic hydroxyl groups formed hydrogen bonds with ASP residues of α-glucosidase. Cultivated T. rupestris (especially foothill-grown) outperformed wild plants in bioactives composition and efficacy, serving as a sustainable alternative. Flavonoids and phenolics contributed to its antidiabetic potential via dual antioxidant and enzyme-inhibitory effects, supporting further pharmaceutical development.
✓ 已验证
DOI
PubMed
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
·
2026
·
IF 5.2
Peiqi Wang,Yan Chen,Jun Wu,Shiqi Jiang,Lu Cao,Ren-ai Xu,Xiaoqun Xu
Bosutinib is a second-generation tyrosine kinase inhibitor (TKI) primarily used for the treatment of chronic myeloid leukemia (CML). The aim of this study was to develop and validate a rapid and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of bosutinib and its major metabolite M5. Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using a gradient elution with acetonitrile and 0.1% formic acid as the mobile phase, and gefitinib was used as the internal standard (IS). Biological analysis showed that both bosutinib (2-400 ng/mL) and its metabolite M5 (1-60 ng/mL) exhibited good linearity in their respective concentration ranges, with correlation coefficients ( r 2 ) of 0.996 and 0.993, respectively. Both of them exhibited intra- and inter-day precision (RSD%) below 15% and accuracy (RE%) within ± 15%. Recoveries were all within the range of 85.3-98.0%, and matrix effects were all within the range of 91.6-101.6%. Ultimately, human liver microsomes (HLM) was used to study in vitro metabolic stability, while in vivo pharmacokinetics were evaluated in rats. In vivo pharmacokinetic studies confirmed that this method could be successfully used for the analysis of bosutinib after oral administration of 50 mg/kg in rats. In vitro results showed that bosutinib had the intrinsic clearance (CL int ) value of 0.03 mL/min/mg and the half-life (t 1/2 ) value of 79.94 min. This study provides a potential reference for the clinical investigation of bosutinib.
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DOI
高影响因子
危险品化学品经营许可证（带存储）