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21.
Nejal M. Bhatt Vijay D. Chavada Mallika Sanyal Pranav S. Shrivastav 《Biomedical chromatography : BMC》2019,33(10)
The present work describes novel methods using densitometry and indirect or off‐line high performance thin‐layer chromatography–mass spectrometry (HPTLC–MS) for the simultaneous detection and quantification of asenapine, propranolol and telmisartan and their phase II glucuronide metabolites. After chromatographic separation of the drugs and their metabolites the analytes were scraped, extracted in methanol and concentrated prior to mass spectrometric analysis. Different combinations of toluene and methanol–ethanol–n‐butanol–iso‐propanol were tested for analyte separation and the best results were obtained using toluene–methanol–ammonia (6.9:3.0:0.1, v/v/v) as the elution solvent. All of the drug–metabolite pairs were separated with a homologous retardation factor difference of ≥22. The conventional densitometric approach was also studied and the method performances were compared. Both of the approaches were validated following the International Conference on Harmonization guidelines, and applied to spiked human plasma samples. The major advantage of the TLC–MS approach is that it can provide much lower limits of detection (1.98–5.83 pg/band) and limit of quantitation (5.97–17.63 pg/band) with good precision (?3.0% coefficient of variation) compared with TLC–densitometry. The proposed indirect HPTLC–MS method is simple yet effective and has tremendous potential in the separation and quantitation of drugs and their metabolites from biological samples, especially for clinical studies. 相似文献
22.
Jing Liu Xiu‐Mei Li Dong‐dong Shi Zhi‐guo Wen Pei‐Long Yang 《Biomedical chromatography : BMC》2019,33(12)
In recent years, the fingerprint of high‐performance liquid chromatography has been extensively applied in the identification and quality control of traditional Chinese medicine. It can be a potential protocol for assessing the authenticity, stability and consistency of traditional Chinese medicine and guaranteeing the expected biological activity. In this paper, a method using high‐performance liquid chromatography to identify and control the quality of the extract of Taraxacum mongolicum Hand.‐Mazz. (TME) was established. With this method, the correlation coefficients of the similarity of 10 batches were ≥0.994. The TME displayed a steady proliferative effect in Lactobacillus plantarum. In brief, this study successfully built a reliable, simple and efficient method to control and confirm the quality and the stability of biological activity of the TME. 相似文献
23.
Xiang Cui Yu‐meng Shen Shu Jiang Da‐wei Qian Er‐xin Shang Zhen‐hua Zhu Jin‐ao Duan 《Journal of separation science》2019,42(8):1520-1527
In this study, a rapid and highly sensitive ultra high performance liquid chromatography with triple quadrupole mass spectrometry method with the mobile phase of acetonitrile and 0.1% aqueous formic acid was established and successfully applied to comparatively analyze main active components after their compatibility. Besides, the effects of Scutellariae Radix, Coptidis Rhizoma and combined extracts on type 2 diabetic rats induced by high‐fat diet along with low dose of streptozocin were investigated. Under the optimized chromatographic conditions, good separation of seven target components was achieved within 12 min. All calibration curves exhibited good linearity (R2 ≥ 0.999). The relative standard deviation of precision, repeatability and stability varied from 0.69 to 2.23, 0.98 to 2.56, and 0.92 to 2.57%, respectively. The recovery ranged from 91.11 to 105.35%. The contents of seven active components were notably reduced after compatibility; however, the hypoglycemic effect of combined extracts was stronger than single drug by decreasing the activities of fructose‐1,6‐bisphosphatase, glucose 6‐phosphatase, phosphoenolpyruvate carboxykinase and increasing the activities of glucokinase, phosphofructokinase, pyruvate kinase. Accordingly, the established analytical method was accurate and sensitive enough for quantitative evaluation of seven investigated compounds. Moreover, the combined extract had definite effects on type 2 diabetes through multiple components against multiple targets. 相似文献
24.
Lana K. Hiscock Brooke M. Raycraft Monika Wałęsa-Chorab Coralie Cambe Alexandre Malinge Prof. Dr. W. G. Skene Hi Taing Prof. Dr. S. Holger Eichhorn Prof. Dr. Louise N. Dawe Prof. Dr. Kenneth E. Maly 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(4):1018-1028
A series of new tetrakis(dialkoxyphenyl) dicyanotetraoxapentacene derivatives ( 1 a – c ) were prepared by reaction of the appropriate terphenyl diols with tetrafluoroterephthalonitrile in good yields. Compounds 1 b and 1 c , which bear hexyloxy and decyloxy side chains, exhibited columnar hexagonal mesophases, as shown by polarized optical microscopy, variable-temperature powder X-ray diffraction, and differential scanning calorimetry. Single-crystal X-ray diffraction of methoxy-substituted 1 a revealed that the dicyanotetraoxapentacene core is highly planar, consistent with the notion that these molecules are able to stack in columnar mesophases. A detailed photophysical characterization showed that these compounds exhibit aggregation-induced emission in solution, emission in nonpolar solvents, weak emission in polar solvents, and strong emission in the solid state both as powder and in thin films. These observations are consistent with a weakly emissive charge-transfer state in polar solvents and a more highly emissive locally excited state in nonpolar solvents. 相似文献
25.
Chaonan Xie Qin Li Gang Han Huan Liu Jien Yang Jincheng Li 《Biomedical chromatography : BMC》2019,33(5)
Tricaine methanesulfonate is one of most commonly used anesthetics in fish during blood sampling, artificial propagation and long‐distance transportation. In this study, an accurate method for the quantitative determination of tricaine in fish samples by a stable isotope dilution assay coupled with high‐performance liquid chromatography–triple quadrupole mass spectrometry was developed. Tricaine‐D5 was synthesized and used as an isotopically labeled internal standard for the determination of tricaine. The analytical performance of the method was validated for tricaine determination in marine fish and freshwater fish. The determination of tricaine was linear in the range of 2.0–200.0 μg L?1. The limit of detection and limit of quantitation for fish muscle tissues were 1.0 and 4.0 μg kg?1, respectively. Good recoveries were obtained in the range of 92.08–97.50%. The inter‐ and intra‐assay relative standard deviations (RSD values) were investigated, and the values were 0.39–3.01 and 0.85–2.77%, respectively. The values of CCα and CCβ were 10.21–10.43 and 10.42–10.87 μg kg?1, respectively. The clearance of MS‐222 from grass carp was further studied using our method. The results demonstrate that MS‐222 could be well absorbed and rapidly eliminated after bath administration. 相似文献
26.
Stanisław A. Różański 《Phase Transitions》2019,92(1):79-86
The volume filling fraction dependence of the effective permittivity of the nematic liquid crystal 4-n-pentyl-4’-cyanobiphenyl embedded in different porous membranes and dispersed with aerosil nanoparticles was determined using broadband dielectric spectroscopy in the frequency range from 106 to 109 Hz. The experimental data were analyzed and compared with some existing theories based on the effective medium approximation and their modifications. The obtained effective permittivities as a function of the volume filling fraction lie between the lower limits of the Wiener and Hashin–Shtrikman bounds. The observed shift of the experimental points reflects the changes in the structure of the investigated composites. 相似文献
27.
Dr. Jun Zeng Dr. Zhichao Wang Dr. Xin Huang Dr. Sabine S. Eckstein Prof. Dr. Xiaohui Lin Prof. Dr. Hailong Piao Prof. Dr. Cora Weigert Dr. Peiyuan Yin Prof. Dr. Rainer Lehmann Prof. Dr. Guowang Xu 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(21):5427-5432
Mass spectrometry (MS) driven metabolomics is a frequently used tool in various areas of life sciences; however, the analysis of polar metabolites is less commonly included. In general, metabolomic analyses lead to the detection of the total amount of all covered metabolites. This is currently a major limitation with respect to metabolites showing high turnover rates, but no changes in their concentration. Such metabolites and pathways could be crucial metabolic nodes (e.g., potential drug targets in cancer metabolism). A stable-isotope tracing capillary electrophoresis–mass spectrometry (CE-MS) metabolomic approach was developed to cover both polar metabolites and isotopologues in a non-targeted way. An in-house developed software enables high throughput processing of complex multidimensional data. The practicability is demonstrated analyzing [U-13C]-glucose exposed prostate cancer and non-cancer cells. This CE-MS-driven analytical strategy complements polar metabolite profiles through isotopologue labeling patterns, thereby improving not only the metabolomic coverage, but also the understanding of metabolism. 相似文献
28.
A series of 3-perfluoroalkylbenzoate esters are synthesised. They tend to exhibit enantiotropic SmA and SmC phases. The clearing points are decreased with increasing the alkoxy chain length and show odd-even effect. With increasing the fluorocarbon chain length, the melting and clearing points increase; however, the SmC phase is suppressed. 相似文献
29.
Mouna Smida Jérome Lhôste Mohamed Dammak Santiago Garcia-Granda 《Arabian Journal of Chemistry》2019,12(8):2519-2523
Crystal structure of Fe2F5(H2O)(Htaz)(taz)(Hdma) which crystallizes in the triclinic system space group with unit cell parameters a = 8.8392(5) Å, b = 9.1948(5) Å, c = 9.5877(5) Å, α = 82.070(3)°, β = 63.699(3)°, γ = 89.202(3)°, Z = 2, and V = 690.91(7) Å3, was synthesized under hydrothermal conditions at 393 K for 72 h, by a mixture of FeF2/FeF3, 1,2,4-triazole molecule (Htaz), and hydrofluoric acid solution (HF 4%) in dimethylformamide solvent (DMF). The main feature of this material is the coexistence of two oxidation states for iron atoms (Fe2+, Fe3+) in the unit cell, which associate by opposite fluorine corners of FeF5N and FeF2N4 octahedra, and/or triazole molecule which originates the 2D produces material. The structure determination, performed from single crystal X-ray diffraction data, lead to the R1/WR2 reliability factors 0.031/0.087. Thermal stability studies (TG/DTG/DTA) show that the decomposition provides in the temperature range 473–773 K and no mass loss was detected before 473 K. Mass spectrometry (MS) has been used. The optical absorption of the solid was measured at the corresponding λmax using UV–vis diffuse-reflectance spectrum. 相似文献
30.
Chunlai Wu Chuanyun Peng 《International journal of environmental analytical chemistry》2019,99(7):670-682
To develop an accurate and precise method for separation and pre-concentration of Hg(II), a novel thionin functionalised core shell structure magnetic material has been prepared and characterised. The extraction ability of the material was evaluated by magnetic solid-phase extraction coupled with inductively coupled plasma mass spectrometry determination of Hg(II) in food and water samples. Combining the advantages of magnetic separation with selective extraction of thionin towards Hg(II), the material exhibits enhanced enrich selectivity and efficiency for Hg(II). The experimental parameters influencing Hg(II) extraction efficiency, including pH of the aqueous solution, the dosage of the adsorbent, extraction time and sample volume, were systematically investigated. Under the optimised conditions, concentration of Hg(II) at 1.0 μg L?1 can be successfully enriched by the material without the interference of the common co-existing ions. The enrichment factor and adsorption capacity were 250 and 75.2 mg g?1, and precise of the method was confirmed by analysing the spiked food, water samples and standard water reference samples with the recoveries of 92.5–101.8%. 相似文献