查找使用阿拉丁产品的科研文献

A comprehensive and high-throughput screening method for multiple prohibited substances by UPLC-QE Plus-HRMS and HPLC-QQQ-MS in human urine for doping control

Yunxi Liu,Tianyu Dong,Kuan Yan,Zhanliang Wang,Genye He,Yufeng Zhang,Congcong Ma,Lu Liu,Wei Chang,Lisi Zhang

Since the World Anti-Doping Agency's (WADA) Prohibited List is updated on an annual basis, screening methods must be continually adapted to align with these changes. In accordance with Technical Document-MRPL 2022, a newly combined, comprehensive, rapid and high-throughput doping control screening method has been developed for the analysis of 350 substances with different polarities in human urine using ultra-high performance liquid chromatography coupled with Q Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer (UPLC-QE Plus-HRMS) and ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometer (UPLC-QQQ-MS). The limits of detection were in the range of 0.12–50 ng mL−1 for beta-2 agonists, hormone and metabolic modulators, narcotics, cannabinoids and glucocorticoids, 0.1–14 ng mL−1 for the manipulation of blood and blood components, beta blockers, anabolic agents and hypoxia-inducible factor (HIF) activating agents, and 2.5–100 000 ng mL−1 for substances of Appendix A, diuretics & masking agents and stimulants. The sample preparation consisted of two parts: one is the dilute & shoot part analyzed in UPLC-QQQ-MS, another is a mixture of the dilute & shoot part and a liquid–liquid extraction part of hydrolyzed human urine analyzed in UPLC-QE Plus-HRMS in full scan mode with polarity switching and parallel reaction monitoring (PRM) mode. The method has been fully validated for doping control purposes. All the substances were compliant with WADA's required 1/2 minimum requirement performance level (MRPL) or minimum reporting level (MRL), and this method was successfully used in the 2022 Beijing Winter Olympic Games and Winter Paralympic Games for anti-doping purpose.

A sensitive and economical method for simultaneous determination of D/L- amino acids profile in foods by HPLC-UV: Application in fermented and unfermented foods discrimination

Li Gao,Piao Xu,Jiaoyan Ren

This work described a sensitive and economical HPLC-UV method with FDAA derivatization to simultaneously detect 36 D/ l -amino acids, which provides higher sensitivity and lower cost than other HPLC-based methods. It was validated for linearity range (8–1000 µmol/L), limits of detection (2.68–62.44 pmol/L), limits of quantification (2.93 to 208.13 pmol/L), intraday precision (0.30 % − 5.31 %), interday precision (1.96 % − 8.04 %) and accuracy (86.53 % − 121.46 %). This method was then applied in the determination of D/L- amino acids abundance in fermented and unfermented food materials and showed the characteristics of each type of foods. The method also demonstrated good performance in another application case for the discrimination of different types of food materials based on D/L- amino acids profile. It emphasizes the ability of the method to study the characteristics, distribution and abundance of d -amino acids in foods and their potential application in food quality control.

The Disappearance Behavior, Residue Distribution, and Risk Assessment of Kresoxim-Methyl in Banana (Musa nana Lour.) Based on a Modified QuEChERS Procedure Using HPLC-MS/MS

Wang Siwei,Sun Haibin,Liu Yanping,Wang Xiaonan,Chang Hong

A modified-QuEChERS method to determine kresoxim-methyl in banana and soil was developed and validated via high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS). The dissipation behavior, residue distribution, and risk assessment of kresoxim-methyl in banana were further investigated based on this method. The dissipation behavior of kresoxim-methyl in banana and soil was described by using first-order kinetics and its half-life, 4.8–5.7 days and 5.5–6.5 days, respectively. The concentrations of kresoxim-methyl were 0.03–0.08 mg kg−1, 0.06–0.17 mg kg−1, and <0.01 mg kg−1 for a whole banana, peel, and pulp, respectively, on the basis of spraying three times the recommended dosage and pre-harvest interval (PHI, 42 days). The results showed that the risk quotient of kresoxim-methyl in banana to people exhibited an acceptable low dietary risk. This current study could help in guiding the scientific and proper usage of this formulation.

Ionic liquid-based dispersive liquid–liquid microextraction followed by dispersive solid phase extraction coupled with HPLC-DAD for the determination of sulfonylurea herbicides in soymilk samples

Jilong Li,Weili Xu,Xiujuan Wang,Fengze Wu,Lin Wang,Ji Feng,Zhibing Wang,Hanqi Zhang

Subzero-temperature homogeneous liquid–liquid extraction for the stereoselective determination of chiral triadimefon and its metabolite in water, fruit juice, vinegar, and fermented liquor by HPLC

Xingle Guo,Haijuan Jiang,Yuqi Guo,Liyan Jia,Xu Jing,Junxue Wu

A novel method based on homogeneous liquid–liquid extraction with deep eutectic solvents (DES) under subzero-temperature conditions in combination with high performance liquid chromatography (HPLC) for the determination of chiral fungicide triadimefon (TF) and its metabolite triadimenol (TN) in water, fruit juice, vinegar, and fermented liquor was developed in this study. The method involved using deep eutectic solvents (DES) under subzero-temperature conditions in combination with high performance liquid chromatography (HPLC). This novel technique, known as subzero-temperature homogeneous liquid–liquid extraction (STHLLE), offers several advantages, including high efficiency, time-saving, low-cost, and eco-friendliness. The enantiomers of chiral TF and TN were simultaneously separated and quantified using HPLC coupled with a Daicel Chiralpak OD-RH column. Various experimental parameters such as DES composition and volume, freezing condition, salt concentration, and pH were optimized to enhance the recoveries of the target analytes. Under the optimized conditions, spiked recoveries of six enantiomers (i.e., S-TF, R-TF, SR-TN, RS-TN, SS-TN, and RR-TN) in the water, fruit juice, vinegar, and fermented liquor samples were 82.2–100.1% with relative standard deviations of 0.4–10.1%. The current method demonstrated a detection range of 0.03–0.06 mg L−1 in the target analytes. This established technique exhibits potential for efficient and precise extraction and quantification of the enantiomers of TF and TN in water phase samples.

Room-temperature synthesis of imine-linked magnetic covalent organic polymers in deep eutectic solvents for the extraction of flavonoids and their determination with HPLC–MS/MS

Bian Yu,Zhang Yuan,Liu Tong,Zhang Feng,Gao Hui-yuan

A novel imine-linked magnetic covalent organic polymer, Fe 3 O 4 @TAB-TFPT, was synthesized using environmentally friendly deep eutectic solvents as the reaction medium instead of conventional organic solvents. The materials were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), FT-IR, N 2 adsorption-desorption isotherms, energy dispersive spectrometer (EDS), X-ray photoelectron spectra (XPS), and thermo gravimetric analysis (TGA). Subsequently, the materials were employed as an adsorbent for magnetic solid-phase extraction (MSPE) of flavonoids, including Kurarinone, Norkurarinone, Xanthohumol, and Isoxanthohumol, prior to their determination by HPLC–MS/MS. The validation results demonstrate good linearity within the concentration range 0.1–1000 ng∙mL −1 ( R 2  ≥ 0.9963), high enrichment factors ranging from 18.9 to 30.7, and low LODs (0.01–0.05 ng∙mL −1 ) and LOQs (0.05–0.1 ng∙mL −1 ). Furthermore, recoveries between 80.60% and 108.40% with relative standard deviations ≤ 8.49% were achieved. The proposed MSPE-HPLC–MS/MS method was successfully applied to the determination of flavonoids in Sophora flavescens Aition sample. Graphical Abstract

Selective Separation and Analysis of Catecholamines in Urine Based on Magnetic Solid Phase Extraction by Mercaptophenylboronic Acid Functionalized Fe3O4-NH2@Au Magnetic Nanoparticles Coupled with HPLC

Qing Han,Xiaoxiao Wu,Yi Cao,Hua Zhang,Yuqin Zhao,Xuejun Kang,Huaiyuan Zhu

A novel magnetic solid phase extraction based on mercaptophenylboronic acid (MPBA)-functionalized Fe3O4-NH2@Au nanomaterial (Fe3O4-NH2@Au-MPBA) was developed for selective separation and enrichment of catecholamines (including dopamine, norepinephrine and adrenaline). Fe3O4-NH2@Au-MPBA nanoparticles were achieved by self-assembly-anchoring MPBA molecules on the surface of Fe3O4-NH2@Au nanocomposites, which were synthesized via a facial ultrasonic auxiliary in situ reduction process. The interaction between cis-diol from catecholamines and boronic acid was reversible and could be flexibly controlled by adjusting pH value. The catecholamines could be quickly adsorbed by Fe3O4-NH2@Au-MPBA in weak alkaline solution (pH 8.0–9.0) and subsequently released in acid solution (pH 1.0–2.0). The process of adsorption and dissociation was very fast. Furthermore, the three catecholamines could be detected in urine from children by high performance liquid chromatography (HPLC) with electrochemical detector. Under optimal conditions, norepinephrine (NE), epinephrine (EP) and dopamine (DA) were separated very well from internal standard and exhibited a good linearity in the range of 2.5–500.0 ng mL−1, with correlation coefficients of r2> 0.9907. Limits of detection (LOD) (signal to noise = 3) were 0.39, 0.27 and 0.60 ng mL−1for NE, EP and DA, respectively. Recoveries for the spiked catecholamines were in the range of 85.4–105.2% with the relative standard deviation (RSD) < 11.5%.Keywords:Fe3O4-NH2@Au;magnetic solid phase extraction;catecholamines;HPLC;electrochemical detection;urine

Fabrication of polyethyleneimine modified magnetic microporous organic network nanosphere for efficient enrichment of non-steroidal anti-inflammatory drugs from wastewater samples prior to HPLC-UV analysis

Xin-Qiao He,Yuan-Yuan Cui,Xiao-Hui Lin,Cheng-Xiong Yang

Development of novel functionalized adsorbents for efficient magnetic solid phase extraction (MSPE) is essential for promoting their versatile applications in sample pretreatment. Herein, we report the fabrication of a new polyethyleneimine-600 decorated magnetic microporous organic network nanosphere (Fe 3 O 4 @MON-PEI 600 ) for effective MSPE of trace non-steroidal anti-inflammatory drugs (NSAIDs) from different water samples. The core-shelled Fe 3 O 4 @MON-PEI 600 integrates the synergistic effects of Fe 3 O 4 , MON and PEI 600 , providing facile and effective extraction to NSAIDs via multiple hydrogen bonding , π-π and hydrophobic interactions. The inner MON shell employs π-π and hydrophobic interaction sites and the outer PEI-600 coat acts as the hydrogen bonding doner/receptor, which affords good extraction performance for NSAIDs. Under optimal conditions, the Fe 3 O 4 @MON-PEI 600 -MSPE-HPLC-UV method gives wide linear range (0.14–400 μg L −1 ), low limits of detection (0.042–0.149 μg L −1 ), good precisions (intra-day and inter-day RSDs < 4.5%, n = 6), and large enrichment factors (97.0–98.2). Extraction mechanisms and selectivity of Fe 3 O 4 @MON-PEI 600 are evaluated in detail. Moreover, Fe 3 O 4 @MON-PEI 600 is successfully applied to enrich the trace NSAIDs in different water samples with the concentrations of 0.7 and 0.8 μg L −1 for 1-naphthylacetic acid, 0.5 and 0.1 μg L −1 for naproxen as well as 0.7 μg L −1 for ibuprofen , respectively. The developed method not only affords a novel and efficient magnetic adsorbent for NSAIDs in aqueous media at trace level, but also provides a new strategy for the rational design and synthesis of multiple functionalized MON composites in sample pretreatment.

Study on the varied content of Polygonatum cyrtonema polysaccharides in the processing of steaming and shining for nine times based on HPLC-MS/MS and chemometrics

Baolei Fan,Guoliang Wei,Xiaofeng Gan,Tingting Li,Zengyi Qu,Sheng Xu,Chao Liu,Chunqi Qian

In this study, we reported the various contents of Polygonatum cyrtonema by extracting polysaccharides (PCPs) using steaming and shining procedures, thus providing scientific basis for the processing of Polygonatum cyrtonema and content analysis of polysaccharides. We established the characteristic fingerprint to identify and analyze polysaccharide component changes in distillated and processed Polygonatum cyrtonema by PMP precolumn derivatization and HPLC-MS/MS technology. We also classified two kinds of solutions by comparing the composition difference of 10 polysaccharide components in the samples with principal component and cluster analysis. There was a huge difference between them and seven monosaccharides. Processed PCPs mainly consisted of galactose along with mannose, followed by glucose. Meanwhile, we found that the results of cluster analysis and principal component analysis were the same. The polysaccharide components extracted from processed Polygonatum cyrtonema and distillate were mainly galactose and mannose. The results of cluster analysis and principal component analysis were the same. The distilled liquid can be divided into 5 categories, and the processed dry extract of Polygonatum cyrtonema can be divided into 4 categories. The changing trend of polysaccharide components of Polygonatum cyrtonema and distilled liquid was revealed during the multiple cycles of steaming and sun drying. The similarity and difference of polysaccharide components in the extracted liquid and the distilled liquid of each batch were shown.

Comparison of three chemometric methods for processing HPLC-DAD data with time shifts: Simultaneous determination of ten molecular targeted anti-tumor drugs in different biological samples

Yue-Yue Chang,Hai-Long Wu,Huan Fang,Tong Wang,Yang-Zi Ouyang,Xiao-Dong Sun,Gao-Yan Tong,Yu-Jie Ding,Ru-Qin Yu

Three intelligent chemometric multi-way calibration methods including alternating trilinear decomposition (ATLD), alternating trilinear decomposition assisted multivariate curve resolution (ATLD-MCR) and multivariate curve resolution-alternating least squares (MCR-ALS) combined with high performance liquid chromatography-diode array detection (HPLC-DAD) were used to quantify ten molecular targeted anti-tumor drugs in three complex biological matrices (plasma, urine and cell culture media matrices). All analytes can be successfully eluted in 6.5 min. In this experiment, various degrees of time shifts occurred in different samples. While slight time shifts exist in the chromatographic analysis , satisfactory results can be obtained by the three proposed methods. When the time shift was large (5.6 s), the average spiked recoveries obtained by ATLD analysis were in the range of 58.9%–116.5%, which was less than satisfactory. However, the average recoveries obtained by MCR-ALS and ATLD-MCR analysis were 89.8%–114.8% and 84.5%–106.1% respectively, and more satisfactory results were obtained. For further research, ATLD-MCR and MCR-ALS methods were compared, and the results were evaluated by statistical tests. Accuracies of concentrations obtained by them were considered to be no significant difference. In addition, compared with other methods currently published, the proposed chemometric methods combined with the HPLC-DAD can rapidly, simultaneously and accurately determine varieties of molecular targeted anti-tumor drugs in different complex biological matrices even in the presence of severe peak overlaps, severe time shifts, slight baseline drifts and different unknown background interferences.

Preparation of magnetic metal organic framework and development of solid phase extraction method for simultaneous determination of fluconazole and voriconazole in rat plasma samples by HPLC

Kamran Bashir,Guoning Chen,Jili Han,Hua Shu,Xia Cui,Lu Wang,Wen Li,Qiang Fu

Fluconazole and voriconazole are the two broad-spectrum triazole antifungals. The present work described the fabrication method for the synthesis of the amino-modified magnetic metal–organic framework. This material was applied as a pre-sample treatment sorbent for the selective extraction of fluconazole and voriconazole in rat plasma samples. The material was fabricated by the chemical bonding approach method and was characterized by different parameters. The factors which affect the extraction efficiency of the sorbent material were also optimized in this study. Due to the optimization of solid-phase extraction conditions, the nonspecific interaction was reduced and the extraction recoveries of target drugs were increased in plasma samples. The extraction method was combined with the HPLC-UV method for the analysis. Excellent linearity (0.1–25 µg/mL), detections (0.02, 0.03 µg/mL) and quantification limits (0.04, 0.05 µg/mL) were resulted for fluconazole and voriconazole respectively. The maximum recoveries from spiked plasma samples of fluconazole and voriconazole were 86.8% and 78.6% and relative standard deviation were 0.9–2.8% and 2.2–3.6% respectively. Moreover, this sorbent material was used multiple times which was an improvement over single-use commercial sorbent materials. This validated method has practical potential for the simultaneous determination of these drugs in therapeutic drug monitoring studies as well as for routine pharmacokinetic evaluations.

HPLC-ESI-qTOF-MS/MS Characterization, Antioxidant Activities and Inhibitory Ability of Digestive Enzymes with Molecular Docking Analysis of Various Parts of Raspberry (Rubus ideaus L.)

Lingfeng Wu,Yufeng Liu,Yin Qin,Lu Wang,Zhenqiang Wu

The anti-oxidative phenolic compounds in plant extracts possess multiple pharmacological functions. However, the phenolic characterization and in vitro bio-activities in various parts of raspberry (Rubus idaeusL.) have not been investigated systematically. In the present study, the phenolic profiles of leaves (LE), fruit pulp (FPE), and seed extracts (SE) in raspberry were analyzed by HR-HPLC-ESI-qTOF-MS/MS method, and their antioxidant activities and digestive enzymes inhibitory abilities were also investigated. The molecular docking analysis was used to delineate their inhibition mechanisms toward type II diabetes related digestive enzymes. Regardless of LE, FPE, or SE, 50% methanol was the best solvent for extracting high contents of phenolic compounds, followed by 50% ethanol and 100% methanol. The LE of raspberry displayed the highest total phenolic content (TPC) and total flavonoid content (TFC). A total of nineteen phenolic compounds were identified. The quantitative results showed that gallic acid, ellagic acid, and procyanidin C3 were the major constituents in the three extracts. The various parts extracts of raspberry all exhibited the strong antioxidant activities, especially for LE. Moreover, the powerful inhibitory effects of the three extracts against digestive enzymes (α-glucosidase andα-amylase) were observed. The major phenolic compounds of the three extracts also showed good inhibitory activities of digestive enzyme in a dose-dependent manner. The underlying inhibitory mechanisms of the main phenolic compounds against digestive enzymes were clarified by molecular docking analysis. The present study demonstrated that the various parts of raspberry had strong antioxidant activities and inhibitory effects on digestive enzymes, and can potentially prevent oxidative damage or diabetes-related problems.Keywords:Rubus idaeusL.;phenolic compounds;HPLC-ESI-HR-qTOF-MS/MS;antioxidant activities;digestive enzymes inhibitors;molecular docking analysis