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Objective:To prepare hollow copper selenide nanoparticles (Cu 2- xSe NPs), and investigate their photothermal properties and radiotherapy sensitization performance. Methods:Hollow copper selenide nanoparticles (Cu 2- xSe NPs) were prepared by sacrificial template method with Cu 2O NPs as sacrificial templates and with selenium powder as selenium source. The surface of copper selenide nanoparticles (Cu 2- xSe NPs) was modified with mercapto-ethylene glycol (mPEG-SH) to obtain Cu 2- xSe-PEG NPs. The morphology, particle size and ultraviolet spectrum of the Cu 2- xSe NPs were characterized by transmission electron microscopy, laser particle size analyzer and ultraviolet spectrophotometer. The photothermal properties and radiosensitization performance of the Cu 2- xSe-PEG NPs were investigated by infrared thermal imager and biological X-ray irradiator. Results:The obtained Cu 2- xSe NPs showed a hollow structure and good monodispersity, and the average diameter were (136.9±7.0) nm. The Cu 2- xSe NPs had absorption in the near-infrared region. When the Cu 2- xSe-PEG NPs sample with the mass concentration of 200 μg/ml were irradiated under 808 nm laser at 1.0 W/cm 2 for 10 min, the temperature raised to more than 55 ℃. The level of reactive oxygen species produced by the Cu 2- xSe-PEG NPs under X-ray irradiation was related to the concentration and radiation dose. Conclusions:The proposed preparation method can control the size of synthesized Cu 2- xSe NPs, and the Cu 2- xSe NPs had good photothermal properties and radiosensitization performance. This work will provide a certain theoretical basis for the application of Cu 2- xSe-PEG NPs in tumor thermoradiotherapy.
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AIM To establish the HPLC fingerprints of flavonoids in Ziziphi spinosae Semen and to determine the contents of two constituents.METHODS With spinosin as a reference peak,the HPLC fingerprints of ten batches of samples were established.The analysis of methanol extract of flavonoids in Ziziphi spinosae Semen was performed on a 30 ℃ thermostatic Agilent TC-C18column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1％ acetic acid flowing at 1 mL/min in a gradient elution manner,and the detection wavelength was set at 280 nm.RESULTS There were ten common peaks in the HPLC fingerprints,eight of which (vicenin-Ⅱ,glucosylvitexin,isospinosin,spinosin,6'-pyridyloylspinosin,6'-p-hydroxybenzoylspinosin,6'-feruloylspinosin and 6'-p-coumaroylspinosin) were identified.Spinosin and 6'-feruloylspinosin showed good linear relationships within the ranges of 15.00-40.00 μg and 5.00-14.00 μg,whose average recoveries (RSDs)were 100.5％ (1.6％) and 100.4％ (1.6％),respectively.CONCLUSION This accurate,simple and reliable method can be used for the quality control of flavonoids in Ziziphi spinosae Semen.
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Deoxyglycychloxazol (TY501) is a glycyrrhetinic acid derivative which exhibits high anti-inflammatory activity and reduced pseudoaldosteronism compared to glycyrrhetinic acid. In this study, a sensitive and rapid liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was established for the quantitation of TY501 in rat plasma. Plasma samples were treated by precipitating protein with methanol and supernatants were separated by a Symmetry C8 column with the mobile phase consisting of me-thanol and 10 mM ammonium formate (containing 0.1%of formic acid) (90:10, v/v). The selected reaction monitoring (SRM) transitions were performed at m/z 647.4-191.2 for TY501 and m/z 473.3-143.3 for astragaloside aglycone (IS) in the positive ion mode with atmospheric pressure chemical ionization (APCI) source. Calibration curve was linear over the concentration range of 5–5000 ng/mL. The lower limit of quantification was 5 ng/mL. The mean recovery was over 88%. The intra-and inter-day precisions were lower than 6.0% and 12.8%, respectively, and the accuracy was within 71.3%. TY501 was stable under usual storage conditions and handling procedure. The validated method has been successfully applied to a pharmacokinetic study after oral administration of TY501 to rats at a dosage of 10 mg/kg.
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<p><b>OBJECTIVE</b>To establish a method for the determination of gypsum and magnesium in decoction by capillary zone electrophoresis and study the influence of different compatibility on the contents of calcium and magnesium dissolution.</p><p><b>METHOD</b>Nine decoctions with gypsum were prepared and analysed by L9 (3(4)) orthogonal design and the contents of calcium and magnesium ions were determined by the set method. The conditions of the experiment were a running buffer of 6.4 mmol x L(-1) imidazole solution (glacial acetic acid ajusted pH to 3.50) and an applied voltage of 10 kV (room temperature). Samples were introduced by hydrodynamic injection (8 cm x 7 s) and determined with on-column UV monitoring at 214 nm. Copper sulphate was chosen as the internal standard.</p><p><b>RESULTS</b>The linear responses covered the range from 0.009 68 mg x L(-1) to 9.68 mg x L(-1) (r = 0.998 1) for calcium, the detection limits (S/N = 3) and the quantitation limits (S/N = 10) of calcium were shown to be 0.002 1 mg x L(-1) and 0.007 1 mg x L(-1), respectively. The average recovery for calcium was 100.4%. The linear response covered the range from 0.01 mg x L(-1) to 10 mg x L(-1) (r = 0.995 9) for magnesium. The detection limits (S/N = 3) and the quantitation limits (S/N = 10) of magnesium showed to be 0.002 8 mg x L(-1) and 0.008 9 mg x L(-1), respectively. The average recovery for magnesium was 96.4%.</p><p><b>CONCLUSION</b>The method is simple, rapid, cost-effective and precise with satisfactory results. The influence of Ephedra and Semen Armeniacae Amarum on the contents of gypsum dissolution are significant, while that of Radix Glycyrrhizae on the contents of gypsum dissolution is insignificant. The influence of Ephedra on the contents of magnesium dissolution are significant, while that of Semen Armeniacae Amarum and Radix Glycyrrhizae on the contents of magnesium dissolution are insignificant.</p>