Quality Inspection and Preparation of Diarrhea Arresting and Dysentery Treating Dietary Traditional Chinese Herbal Medicine for Livestock

[Objective] This study was aimed to formulate the quality inspection of diarrhea arresting and dysentery treating dietary traditional Chinese herbal medicines for livestock.[Methods] Physiochemical identification and contrast test of UV spectrophotometer qualitative detection were adopted.[Results] The difference in the peak value of maximum adsorption peak detected by diluted water method was greater than 1 nm; the maximum adsorption peak values obtained by the 0.9％ hydrochloric acid and 60％ ethanol methods had a difference of less than 1 nm,and the secondary adsorption peak values also had a difference of less than 1 nm.[Conclusion] The 0.9％ hydrochloric acid and 60％ ethanol methods were selected as the quality inspection standards for the preparation of diarrhea arresting and dysentery treating dietary traditional Chinese herbal medicines for livestock.

Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry

In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation of impurity profile in moxifloxacin （MOX） drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.

Increase in functional groups for POSS by introducing branched phenylglycidylether

In the selected experimental conditions, firstly, the branched products with functional groups, N-（2-hydroxylpropylphenylether） （3-aminopropyl） triethoxysilane （APES-PGE, containing one hydroxyl group） and N-[di（2-hydroxylpropylphenylether）]（3-aminopropyl） triethoxysilane （APES-PGE2, containing two hydroxyl groups）, were synthesized by reacting 1 mole of （3-aminopropyl）triethoxysilane （APES） with 2 mole of phenylglycidylether （PGE）. Then the hydrolytic condensation of APES-PGE and APES-PGE2 was performed by dissolving 1 g of the corresponding silane in 1.5 ml tetrahydrofuran （THF）, adding water and eventually a catalyst （molar ratios: [H2O]/Si=3, [NaOH]/Si=0.05）, and heating at 50 ℃ for 24 h, allowing continuous evaporation of volatiles. The final products with branches containing hydroxyl groups were polyhedral oligomeric silsesquioxanes （POSS）. The products from two reactions were characterized by standard spectroscopic techniques, gel partition chromatography （GPC）, Fourier-transformed infrared spectroscopy （FTIR） and matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry （UV-MALDI-TOF MS）. Additionally, a narrow mass distribution of multifunctionalized POSS was shown by UV-MALDI-TOF MS and assignments of the MS peaks.

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading, washing, and eluting） used a flow rate of1.0 m L/min, and dicyandiamide was eluted with 20 m L of a methanol/acetonitrile mixture（V/V = 2：3）, followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy（HPLC–UV）. Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge（with activated carbon）.Separation was achieved on a ZIC-Hydrophilic Interaction Liquid Chromatography（ZIC-HILIC）（50 mm × 2.1 mm, 3.5 μm） chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions（R^2〉 0.999）. Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations（RSDs, n = 3） were below 6.1% with a detection limit of 5.0 ng/m L for stream water samples.

Elucidating the various multi-phosphorylation statuses of protein functional regions by 193-nm ultraviolet photodissociation

Ultraviolet photodissociation is a high-energy fast excitation method in mass spectrometry and has beensuccessfully applied for the elucidation of sequences and structures of biomolecules. However, its abilityto distinguish the phosphorylation sites isomers of multi-phosphopeptides has been not systematicallyinvestigated until now. A 193-nm ultraviolet laser dissociation mass spectrometry system wasestablished in this study and applied to elucidate the complex multi-phosphorylation statuses mimickingthe functional regions of Sicl, Gli3 and Tau. The numbers of matched fragment ions and phosphorylationsite-determining ions were improved on average 123% and 104%, respectively, by utilizing the ultravioletphotodissociation strategy, comparing to the typically utilized collision induced dissociation strategy.Finally. 94% phosphorylation sites within various statuses were unambiguously elucidated.