JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Jiatai Yin,Yiheng Gou,Yiheng Wang,Qingyuan Ma,Rui Wang,Jing Yu,Yajun Zhang,Jing Wang,Qian Li,Xinfeng Zhao
Epimer separation is crucial in the field of analytical chemistry, separation science, and the pharmaceutical industry. No reported methods could separate simultaneously epimers or even isomers and remove other unwanted, co-existing, interfering substances from complex systems like herbal extracts. Herein, we prepared a heptapeptide-modified stationary phase for the separation of 1R,2S -(-)-ephedrine [(-)-Ephe] and 1S,2S -(+)-pseudoephedrine [(+)-Pse] epimers from Ephedra sinica Stapf extract and blood samples. The heptapeptide stationary phase was comprehensively characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy. The separation efficiency of the heptapeptide column was compared with an affinity column packed with full-length β 2 -AR functionalized silica gel (β 2 -AR column). The binding affinity of the heptapeptide with (+)-Pse was 3-fold greater than that with (-)-Ephe. Their binding mechanisms were extensively characterized by chromatographic analysis, ultraviolet spectra, circular dichroism analysis, isothermal titration calorimetry, and molecule docking. An enhanced hydrogen bonding was clearly observed in the heptapeptide-(+)-Pse complex. Such results demonstrated that the heptapeptide can recognize (+)-Pse and (-)-Ephe epimers in a complex system. This work, we believe, was the first report to simultaneously separate epimers and remove non-specific interfering substances from complex samples. The method was potentially applicable to more challenging sample separation, such as chiral separation from complex systems.
研究领域:
分析化学
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药学
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生物化学
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产品关联
DOI
PubMed
高影响因子
Current Analytical Chemistry
·
2023
·Vol. 19
·期 9
·685-692
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IF 1.8
Xu Jinqiu,Gong Yinhua,Huang Rongrong,Cai Liangliang,Ma Xiaofei
Background: In borax buffer, ephedrine (EPH) and pseudoephedrine (PSE) can be well separated (Rs>10) in capillary electrophoresis (CE) without adding any other compounds, but the specific mechanism remains unclear. Methods: Titration analysis, nuclear magnetic resonance analysis,
mass spectrum analysis and molecular modeling were used to investigate the separation mechanism. Results: Tetrahydroxy borate (a hydrolyzate of borax or boric acid) could react with ephedrine and pseudoephedrine to form self-assembled complexes, but the two complexes had different stabilities
and electrophoretic mobilities resulting from the different steric configurations of analytes. Conclusion: The complexation based on borax was responsible for the separation.
研究领域:
分析化学
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药学
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DOI
高影响因子
SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
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2021
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IF 4.098
Yuhui Zhang,Xuanping Tan,Ligang Xing,Huan Wu,Jidong Yang
Two chiral drugs, ephedrine (EH) and pseudoephedrine (PEH), were commonly used in clinical treatment. Ephedrine (EH) and pseudoephedrine (PEH) could make different changes in resonance Rayleigh scattering spectrum of the detection system which use Ce 3+ functionalized gold nanoparticles as probe. Therefore, a new method of detecting EH and PEH separately was developed. The RRS spectrum and UV–Vis absorption spectrum of AuNPs-Ce 3+ detection system was analyzed in order to discuss the mechanism. Under optimal experimental conditions, the linear range of EH and PEH were 20–920 ng/mL and 40–520 ng/mL, respectively. The detection limit were 1.9 ng/mL and 3.8 ng/mL, respectively. Last used for actual testing, this method had obtained good results.
研究领域:
分析化学
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药物分析
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生物医学
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DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
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2022
·Vol. 37
·期 2
·e5541
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IF 1.911
Yongjing Liu,Suxia Zhang,Li Lou,Tang Yan,Wei Xu
In this study, deep eutectic solvent (DES), as a new green solvent, was used to extract bioactive alkaloids from Ephedrae Herba using supersonic extraction. In a variety of tested hydrophilic and hydrophobic DESs, DES composed of choline chloride and xylitol was proved to be the most efficient solvent. Factors affecting extraction efficiency, including the mole ratio of hydrogen bond acceptor/hydrogen bond donor, water contention, and solid/liquid ratio, were optimized individually. Under optimal conditions, the yield of ephedrine (EP) and pseudoephedrine obtained using this new method was 14.24 and 4.32 mg/g, respectively, which was higher than that using the traditional solvent (acidified water and methanol). Furthermore, the extraction mechanism of DES and EP was investigated using molecular dynamics simulation study. Structural properties such as radial distribution functions and average number of hydrogen bonds were then computed. The results showed that hydrogen bonds and van der Waals forces are important driving forces of extraction; in addition, the hydrogen bonds between the Cl atom of choline chloride and N atom of EP played a dominant part in the extraction process. Based on the extraction principle, the extraction method using choline chloride as extraction solvent was also discussed.
研究领域:
药学
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分析化学
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绿色化学
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
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2022
·Vol. 23
·期 18
·10898
·
IF 6.208
Chenchen Guo,Ying Chen,Dengyun Wu,Yu Du,Mengyue Wang,Cunqi Liu,Jianzhou Chu,Xiaoqin Yao
Pinellia ternata(Thunb.) Druce is a traditional medicinal plant containing a variety of alkaloids, which are important active ingredients. Brassinolide (BR) is a plant hormone that regulates plant response to environmental stress and promotes the accumulation of secondary metabolites in plants. However, the regulatory mechanism of BR-induced alkaloid accumulation inP. ternatais not clear. In this study, we investigated the effects of BR and BR biosynthesis inhibitor (propiconazole, Pcz) treatments on alkaloid biosynthesis in the bulbil ofP. ternata. The results showed that total alkaloid content and bulbil yield was enhanced by 90.87% and 29.67% under BR treatment, respectively, compared to the control. We identified 818 (476 up-regulated and 342 down-regulated) and 697 (389 up-regulated and 308 down-regulated) DEGs in the BR-treated and Pcz-treated groups, respectively. Through this annotated data and the Kyoto encyclopedia of genes and genomes (KEGG), the expression patterns of unigenes involved in the ephedrine alkaloid, tropane, piperidine, pyridine alkaloid, indole alkaloid, and isoquinoline alkaloid biosynthesis were observed under BR and Pcz treatments. We identified 11, 8, 2, and 13 unigenes in the ephedrine alkaloid, tropane, piperidine, and pyridine alkaloid, indole alkaloid, and isoquinoline alkaloid biosynthesis, respectively. The expression levels of these unigenes were increased by BR treatment and were decreased by Pcz treatment, compared to the control. The results provided molecular insight into the study of the molecular mechanism of BR-promoted alkaloid biosynthesis.Keywords:alkaloid;brassinolide;ephedrine;secondary metabolism;RNA-seq
研究领域:
植物学
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药理学
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分子生物学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2022
·Vol. 45
·期 5
·1051-1058
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IF 3.614
Chunying Song,Dongping Yu,Gaowa Jin,Junjie Ding,Han Zhou,Zhimou Guo,Xinmiao Liang
Ephedrae Herba is one of the most commonly used herbal medicines, and it has been shown that most of the clinical efficacy for cold and asthma is exerted by its alkaloidal components. A simple and sensitive high-performance liquid chromatography method was developed using a perfluorooctyl column for the simultaneous determination of five alkaloids (norephedrine, norpseudoephedrine, ephedrine, pseudoephedrine, and methylephedrine) in Ephedrae Herba . The mobile phase comprising acetonitrile and 15 mM ammonium trifluoroacetate was used to elute the targets in isocratic elution mode. The method was validated for linearity ( R 2 > 0.999), repeatability, intraday and interday precision, recoveries with trueness (93.87–110.99%), limits of detection (5.35–5.76 µg/mL), and limits of quantification (20 µg/mL). The quantitative results revealed that the developed method was precise and accurate. Then it was successfully applied to determine the difference in the contents of three batches of Ephedrae Herba from three pharmaceutical companies.
研究领域:
药学
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分析化学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2021
·
IF 4.821
Ling Jia,Yue Mao,Siqi Zhang,Hong Li,Ming Qian,Dongbo Liu,Bin Qi
An electrochemical switch sensor toward ephedrine hydrochloride (EPh) determination was developed based on complex reactions and molecular imprinting (MIP) technique. The MIP was formed on a glassy carbon electrode (GCE) modified with Nafion-multi-walled carbon nanotube (Nafion-MWCNTs/GCE). The analytical performances of this sensor were evaluated using several electrochemical methods by measuring the response of EPh elution and re-adsorption in MIP. The working concentration range of this sensor was 1.8 × 10 −7 mol/L ~ 7.5 × 10 −5 mol/L with a detection limit of 7.2 × 10 −8 mol/L (S/N = 3). The sensor also displayed a fast response time of less than 180 s and good anti-interference ability towards several co-existing substances. The determination of EPh in spiked Saliva samples also receives satisfying results which suggest potential applications of the present sensor.
研究领域:
分析化学
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药物分析
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电化学
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产品关联
DOI
高影响因子
ANALYST
·
2023
·Vol. 148
·期 6
·1322-1329
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IF 4.2
Chunyan Zhang,Yifeng Fan,Liangliang Cai,Xiaofei Ma
The discovery of novel chiral selectors always fascinates us. This work describes the chiral separation performances of a new chiral selector (kasugamycin, KAS) in capillary electrophoresis (CE) for six pairs of stereoisomers, including ephedrine and pseudoephedrine, quinine and quinidine, cinchonine and cinchonidine, and amlodipine, promethazine and ofloxacin enantiomers. Kasugamycin, an aminoglycoside antibiotic in agriculture, shows significant biological activity against rice blast with low toxicity. As it turns out, this new chiral selector possesses good CE compatibility and stereoselectivity towards model analytes. In this work, we systematically investigated several separation parameters including kasugamycin concentration, buffer pH, separation voltage and the composition of the buffer solution. A detailed discussion about the chiral recognition mechanism was made based on Statistical Product and Service Solution (SPSS) analysis, NMR experiments (1D and 2D) and molecular modeling. This is the first time that kasugamycin is utilized as a chiral selector in CE, and the development of new chiral selectors from agricultural or veterinary antibiotics deserves more attention.
研究领域:
分析化学
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药学
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色谱学
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农业化学
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产品关联
DOI
PubMed
高影响因子
PHYTOCHEMICAL ANALYSIS
·
2019
·Vol. 31
·期 2
·242-251
·
IF 1.963
Luwei Fang,Jinfeng Xie,Liangwen Lin,Minglei Tian,Kyung Ho Row
Introduction Ephedrine is a typical compound found in lots of plant species that is used in several medicines for the treatment of asthma and bronchitis. However, excess amounts are harmful to humans, so it needs to be removed. Objective This study developed a multi-phase extraction (MPE) method with a molecular imprinted polymer (MIP) coated ionic liquid (IL)-based silica (SiO 2 @IL@MIP) to simultaneously extract and separate ephedrine from Pinellia ternata , 10 medicines, and urine samples. Methods IL was immobilized on silica. Subsequently, the IL was combined with the functional monomer, followed by the addition of the crosslinker and template. The resulting sorbent was applied to the MPE, and the extraction, washing and elution solvents were evaluated. Results Fourier-transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the synthesis of SiO 2 @IL@MIP. A maximum adsorption amount of 5.76 mg/g was obtained at 30°C at a neutral pH. In MPE, 10.00 mL of methanol could extract all the ephedrine from Pinellia ternata . The interference was removed by washing with 4.00 mL of water, ethanol, and acetonitrile. Finally, 8.00 mL of methanol/acetic acid (99:1, v / v ) was applied as the elution solvent. The following were extracted: 5.50 μg/g of ephedrine from Pinellia ternata , 0.00–46.50 μg/g from the 10 herbal medicines, and 68.70–102.80 μg/mL in the urine samples. Conclusion The proposed method was applied successfully to the simultaneously extraction and separation of ephedrine from plants and medicines. These results are expected to provide important data for the development of new methods for the separation and purification of bioactive compounds.
研究领域:
分析化学
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药学
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植物化学
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分离科学
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产品关联
DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2024
·Vol. 38
·期 20
·e9877
·
IF 1.8
Yiqin Xu,Fang Yang,Hong Ye,Qingqiang Tang,Yanwen Chen,Zhigang Gao,Shuhua Wang,Fang Zhang,Xiaojing Li
Rationale In recent years, ephedrine psychoactive substances have attracted much attention due to their prevalence in water bodies and potential threat to aquatic ecosystems. Psychoactive substances have been considered as a new type of environmental pollutant due to their unpredictable potential risks to the behavior and nervous system of non-target organisms. A rapid, sensitive, selective, and robust method for the quantification of three ephedrine psychoactive substances in sewage is needed. Methods An ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of three ephedrine psychoactive substances in water. The optimal processing conditions were determined by optimizing the chromatography—mass spectrometry and solid-phase extraction (SPE) conditions (e.g., the SPE column, sample pH, washing, and elution), and the treatment conditions were determined; this was achieved via positive ion scanning in multiple reaction monitoring mode. Poly-Sery MCX was selected as the extraction column, with samples loaded at pH 3. And 4-mL solution of 2% formic acid (FA) aqueous solution was used as the eluent; the target compounds were eluted with 5 mL of 5% NH 4 OH in acetonitrile (ACN) solution. The best results were obtained when the residue was resolubulization in ACN after nitrogen evaporation. Results The developed UPLC-MS/MS showed a good linear relationship in the range of 0–50.00 μg/L, with determination coefficients ( R 2 ) greater than 0.9990. The detection limit and quantitation limit were 0.05–0.10 and 0.20–0.50 μg/L, respectively. Recovery rates of the target compounds in blank sewage at three different concentrations ranged from 92.37% to 106.31%, with relative standard deviations (RSDs) of 0.77%–4.83% (n = 7). Conclusions This method has been successfully applied to the analysis of surface water and domestic sewage, and the samples were processed stably, indicating that the method is practical for the determination of ephedrine psychoactive drugs in water bodies.
研究领域:
环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Engineering
·
2021
·
IF 7.553
Lu Zhao,Hao Liu,Yingchao Wang,Shufang Wang,Dejin Xun,Yi Wang,Yiyu Cheng,Boli Zhang
Xuanfeibaidu Formula (XFBD) is a Chinese medicine used in the clinical treatment of coronavirus disease 2019 (COVID-19) patients. Although XFBD has exhibited significant therapeutic efficacy in clinical practice, its underlying pharmacological mechanism remains unclear. Here, we combine a comprehensive research approach that includes network pharmacology, transcriptomics, and bioassays in multiple model systems to investigate the pharmacological mechanism of XFBD and its bioactive substances. High-resolution mass spectrometry was combined with molecular networking to profile the major active substances in XFBD. A total of 104 compounds were identified or tentatively characterized, including flavonoids, terpenes, carboxylic acids, and other types of constituents. Based on the chemical composition of XFBD, a network pharmacology-based analysis identified inflammation-related pathways as primary targets. Thus, we examined the anti-inflammation activity of XFBD in a lipopolysaccharide-induced acute inflammation mice model. XFBD significantly alleviated pulmonary inflammation and decreased the level of serum proinflammatory cytokines. Transcriptomic profiling suggested that genes related to macrophage function were differently expressed after XFBD treatment. Consequently, the effects of XFBD on macrophage activation and mobilization were investigated in a macrophage cell line and a zebrafish wounding model. XFBD exerts strong inhibitory effects on both macrophage activation and migration. Moreover, through multimodal screening, we further identified the major components and compounds from the different herbs of XFBD that mediate its anti-inflammation function. Active components from XFBD, including Polygoni cuspidati Rhizoma , Phragmitis Rhizoma , and Citri grandis Exocarpium rubrum , were then found to strongly downregulate macrophage activation, and polydatin, isoliquiritin, and acteoside were identified as active compounds. Components of Artemisiae annuae Herba and Ephedrae Herba were found to substantially inhibit endogenous macrophage migration, while the presence of ephedrine, atractylenolide I, and kaempferol was attributed to these effects. In summary, our study explores the pharmacological mechanism and effective components of XFBD in inflammation regulation via multimodal approaches, and thereby provides a biological illustration of the clinical efficacy of XFBD.
研究领域:
药理学
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免疫学
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转录组学
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中医药
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生物化学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）