1.Liquisolid technique for enhancement of dissolution prosperities of tanshinone II(A).
Xiao-qian LIU ; Qing-ju MENG ; Xue-lin XU ; Jie ZHAO ; Hua YANG ; Hong YI
China Journal of Chinese Materia Medica 2015;40(24):4840-4846
The technique of liquisolid compress is a new technique developed in 1990s, which was considered to be the most promising technique to improve the dissolution of water-insoluble drugs. In this article, tanshinone II(A) and the extracts of the ester-solubility fractions were chosen as the model drugs to evaluate the effects of the liquisolid technique for enhancement of dissolution properties of tanshinone II(A). Several liquisolid tablets (LS) formulations containing different dosage of drugs and various liquid vehicle were pre-pared and for all the formulations, microcrystalline cellulose and silica were chosen as the carrier and coating materials to evaluate their flow properties, such as angle of repose, Carr's compressibility index and Hausner's ratio. The interaction between drug and excipients in prepared LS compacts were studied by differential scanning calorimetry(DSC) and X-ray powder diffraction (XRPD). The dissolution curves of tanshinone II(A) from liquisolid compacts were investigated to determine the technique's effect in improving the dissolution of tanshinone II(A) and its impacting factors. According to the results, the dissolution increased with the rise in the dissolution of the liquid-phase solvent. The R-value and drug dosage can significantly affect the drug release, but with less impact on active fractions. This indicated that liquisolid technique is a promising alternative for improvement of dissolution property of water-soluble drugs, and can make a synergistic effect with other ester-soluble constituents and bettern improve the release of tanshinone II(A). Therefore, the technique of liquisolid compress will have a better development prospect in traditional Chinese medicines.
Calorimetry, Differential Scanning
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Diterpenes, Abietane
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chemistry
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Solubility
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X-Ray Diffraction
2.Effects of micronization on micromeritics properties of baicalin.
Hong-Mei YAN ; Dong-Mei DING ; E SUN ; Jing WANG ; Xiao-Bin JIA ; Zhen-Hai ZHANG
China Journal of Chinese Materia Medica 2014;39(4):653-656
Baicalin extremely fine powder was made by using ball-mill and the effect of micronization on the micromeritics properties of baicalin was studied and analyzed. The microstructures of baicalin ordinary and extremely fine powder were compared by scanning electron microscope, differential scanning calorimeter and X-ray diffraction and the powder characteristic of them was investigated. The hygroscopicity was studied. The effect of micronization on the dissolution of baicalin was investigated. The results showed that the chemical constituents of baicalin were not changed after micronization with better compressibility. It was confirmed that micronization technology had a certain application value in promoting the insoluble component of baicalin absorption with higher dissolution.
Calorimetry, Differential Scanning
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Drugs, Chinese Herbal
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chemistry
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Flavonoids
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chemistry
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Particle Size
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Solubility
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Wettability
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X-Ray Diffraction
3.Polymorphism of the 5R-5-hydroxytriptolide.
Rui-li LIU ; Ya-xi YANG ; Dong-ying CHEN
Acta Pharmaceutica Sinica 2011;46(11):1357-1360
5R-5-hydroxytriptolide (LLDT-8) is a new drug candidate which is in clinical trial treating rheumatoid arthritis. Polymorph screening of the compound was carried out in this study. Polymorph of LLDT-8 was prepared by evaporative crystallization and antisolvent crystallization methods and was characterized by powder X-ray diffraction (p-XRD), infrared spectrometry (IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TG). It was found that p-XRD patterns, DSC curves, TG curves and IR spectra of the LLDT-8 samples prepared by the above recrystallization methods were all consistent. The 20 of main peaks in the p-XRD patterns appeared at 7.58 degrees, 8.14 degrees, 8.66 degrees, 15.46 degrees, 16.46 degrees, 29.54 degrees, 31.16 degrees and 38.26 degrees, while the infrared absorption peaks appeared at 3 471.3, 2 962.2, 2 887.0, 1 762.6, 1 677.8, 1 432.9, 1 365.4, 1 247.7, 1 080.0, 1 031.7 and 877.5 cm(-1). LLDT-8 was decomposed at 271.2 degrees C based on the determination from DSC and TG. It was showed in single crystal X-ray diffraction study that LLDT-8 crystal was monoclinic with the space group being P2 (1). The cell parameters were found to be: a = 11.460 1 (11), b = 6.320 5 (6), c = 13.028 1 (12), alpha = 90.00, beta = 115.557 (2) and gamma = 90.00. The crystal was a hydrogen-bonded dimmer. The slurry experiments, which were further conducted in solvents with different polarities, confirmed the stability of solid state of LLDT-8 based on the p-XRD determination. The polymorph of LLDT-8 made assurance of its efficacy consistence during its clinical trials.
Calorimetry, Differential Scanning
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Crystallization
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Diterpenes
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chemistry
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Drug Stability
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Spectrophotometry, Infrared
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Thermogravimetry
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X-Ray Diffraction
4.Structure charateristics of mitoxantrone transforsomes.
Tong CHEN ; Shixiang HOU ; Biqiong SHI ; Yu ZHENG ; Yiyi SUN ; Yunfei TIAN
Journal of Biomedical Engineering 2005;22(3):555-559
This study sought to clarify the molecular location and the interaction between mitoxantrone and mitoxantrone transforsomes. The anthraquinone of mitoxantrone, a heterocyclic ring that intercalates in the lipid of bilayer, was determined by UV-spectrophotometry and electron probes scan microscopy. Two aminoethylamino side-chains of the drugs fit to the phosphates of lecithin were determined by 8-value, thus the interaction with lecithin was substantiated. Differential scanning calorimetry confirmed that mitoxantrone has remarkable stabilizing effect on the mitoxantrone transforsomes membrane. The mitoxantrone binds tightly to lecithin. So a high degree of encapsulation efficiency and the sustained-release character of mitoxantrone transforsomes are verified.
Anthraquinones
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chemistry
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Calorimetry, Differential Scanning
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Delayed-Action Preparations
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chemistry
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Lecithins
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chemistry
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Mitoxantrone
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chemistry
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Spectrophotometry
5.Study on identification of four kinds of Gentianaceae Mongolian medicine Digeda with spectroscopy techniques.
Li-juan LV ; Yong-hui GUO ; Ya-chan ZHAO ; Dong-dong ZHAO ; Min-hui LI
China Journal of Chinese Materia Medica 2015;40(5):799-803
To study the identification of Gentianaceae Mongolian medicine Digeda with spectroscopy techniques, near infrared spectroscopy and differential scanning calorimetry techniques were applied to study on the identification of 4 kinds of Gentianaceae Mongolian medicine Digeda, and characteristic spectrums obtained were systematically analyzed. In NIR study, the four species of Digeda exist some differences in 4 250-4 400 cm(-1) and 5 650-5 800 cm(-1) of one-dimensional spectra, and show significant differences in 4 100- 4 400 cm(-1), 4 401-4 900 cm(-1) and 5 400-5 800 cm(-1) of the second derivative spectra. DSC curves of them present distinct topological pattern, characteristic peak and peak temperature. Using near infrared spectroscopy and differential scanning calorimetry analysis can realize efficient and accurate identification of four kinds of Mongolian medicine Digeda, and provide scientific basis for the efficient and accurate identification of other Gentianaceae Mongolian medicine Digeda.
Calorimetry, Differential Scanning
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methods
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China
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Gentianaceae
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chemistry
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classification
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Medicine, Mongolian Traditional
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Spectroscopy, Near-Infrared
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methods
6.Effect of glyceryl triacetate on properties of PLA/PBAT blends.
Nan YANG ; Xiyuan WANG ; Yunxuan WENG ; Yujuan JIN ; Min ZHANG
Chinese Journal of Biotechnology 2016;32(6):839-847
Poly lactic acid (PLA)/Poly (butyleneadipate-co-terephthalate)(PBAT) and glyceryl triacetate (GTA) blend were prepared by torque rheometer, and the effect of GTA on thermodynamical performance, mechanical properties and microstructure of PLA/PBAT composites were studied using differential scanning calorimeter(DSC), dynamic mechanical analysis(DMA), universal testing machine, impact testing machine and scanning electron microscope(SEM). After adding GTA, Tg values of the two phases gradually became closer, blends cold crystallization temperature and melting temperature decreased. When with 3 phr GTA, the dispersed phase particle size of PLA/PBAT blend decreased. Mechanics performance test showed that the elongation at break and impact strength of the PLA/PBAT blend was greatly increased with 3 phr GTA, and the elongation at break increased 2.6 times, improved from 17.7% to 64.1%.
Acetates
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chemistry
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Calorimetry, Differential Scanning
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Crystallization
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Lactic Acid
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Polyesters
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chemistry
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Polymers
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Temperature
7.Phase transformation analysis of varied nickel-titanium orthodontic wires.
Chao-chao REN ; Yu-xing BAI ; Hong-mei WANG ; Yu-feng ZHENG ; Song LI
Chinese Medical Journal 2008;121(20):2060-2064
BACKGROUNDThe shape memory effect of nickel-titanium (NiTi) archwires is largely determined by the phase transition temperature. It is associated with a reversible transformation from martensite to austenite. The aim of this study was to characterize austenite, martensite and R phase temperatures as well as transition temperature ranges of the commonly used clinical NiTi orthodontic arch wires selected from several manufacturers.
METHODSDifferential scanning calorimetry (DSC) method was used to study the phase transformation temperatures and the phase transition processes of 9 commonly used clinical NiTi alloys (types: 0.40 mm (0.016 inch), 0.40 mm x 0.56 mm (0.016 inch x 0.022 inch)).
RESULTSThe austenite finish temperatures (Af) of 0.40 mm Smart, Ormco and 3M NiTi wires were lower than the room temperature, and no phase transformation was detected during oral temperature. Therefore, we predicted that these types of NiTi did not possess shape memory property. For 0.40 mm and 0.40 mm x 0.56 mm Youyan I NiTi wires, no phase transformation was detected during the scanning temperature range, suggesting that these two types of wires did not possess shape memory either. The Af of 0.40 mm x 0.56 mm Smart, L&H, Youyan II Ni-Ti wires were close to the oral temperature and presented as martensitic-austenitic structures at room temperature, suggesting the NiTi wires listed above have good shape memory effect. Although the 0.40 mm x 0.56 mm Damon CuNiTi wire showed martensitic-austenitic structures at oral temperature, its Af was much higher than the oral temperature. It means that transformation from martensite to austenite for this type of NiTi only finishes when oral temperature is above normal.
CONCLUSIONThe phase transformation temperatures and transformation behavior varied among different commonly used NiTi orthodontic arch wires, leading to variability in shape memory effect.
Calorimetry, Differential Scanning ; Dental Alloys ; chemistry ; Nickel ; chemistry ; Orthodontic Wires ; Temperature ; Titanium ; chemistry
8.Detection of crystal polymorphs of nateglinide by DSC.
Ke-jiang LIN ; Wei CHEN ; Qi-dong YOU
Acta Pharmaceutica Sinica 2002;37(1):46-49
AIMTo establish the differential scanning calorimetric (DSC) methodology for controlling the crystal-type B form of nateglinide.
METHODSAccurately weighed pure dried (P2O5 as desiccant for 4 h at 80 degrees C in vacuum) fine powder of crystal-type B and H of nateglinide were measured dQ/dT by DSC at heating rate of 10 degrees C. min-1 and temperature between 100 degrees C and 200 degrees C to calculate the enthalpy delta HB and delta HH. Accurately weight a series of uniform mixtures of crystal-type B and H of dried fine powder of nateglinide in different proportions. The enthalpy of the mixtures is measured by DSC as above to calculate the enthalpy (sigma delta H). Using B% as X, sigma delta H as Y, the regression equation was obtained. According to this equation, the unknown composition of mixed crystal was evaluated by the sigma delta H values. The method was used to control the limitation of crystal-type B of nateglinide by the sigma delta H value of mixture of known composition as reference.
RESULTSThe results measured from different laboratories showed that the repeatability was 0.61% and the recoveries were 86.2%-127% when the amounts of crystal-type B were between 0-15%.
CONCLUSIONThis method can be used to evaluate the crystal-type B composition of nateglinide.
Calorimetry, Differential Scanning ; Crystallization ; Cyclohexanes ; chemistry ; Phenylalanine ; analogs & derivatives ; chemistry ; Quality Control
9.In vitro study on exothermic reaction of polymer-based provisional crown and fixed partial denture materials measured by differential scanning calorimetry.
Mun Jeung KO ; Ah Ran PAE ; Sung Hun KIM
The Journal of Korean Academy of Prosthodontics 2006;44(6):690-698
STATEMENT OF PROBLEMS: The heat produced during polymerization of polymer-based provisional materials may cause thermal damage to the vital pulp. PURPOSE: This study was performed to evaluate the exotherm reaction of the polymerbased provisional materials during polymerization by differential scanning calorimetry and to compare the temperature changes of different types of resins. MATERIAL AND METHODS: Three dimethacrylate-based materials (Protemp 3 Garant, Luxatemp Plus, Luxatemp Fluorescence) and five monomethacrylate-based material (Snap, Alike, Unifast TRAD, Duralay, Jet) were selected. Temperature changes of polymer-based provisional materials during polymerization in this study were evaluated by D.S.C Q-1000 (TA Instrument, Wilmington, DE, USA). The following three measurements were determined from the temperature versus time plot: (1) peak temperature, (2) time to reach peak temperature, (3) heat capacity. The data were statistically analyzed using one-way ANOVA and multiple comparison Bonferroni test at the significance level of 0.05. RESULTS: The mean peak temperature was 39.5 degrees C (+/- 1.0). The peak temperature of the polymer-based provisional materials decreased in the following order: Duralay > Unifast TRAD, Alike > Jet > Luxatemp Plus, Protemp 3 Garant, Snap, Luxatemp Fluorescence. The mean time to reach peak temperature was 95.95 sec (+/- 64.0). The mean time to reach peak temperature of the polymer-based provisional materials decreased in the following order: Snap, Jet > Duralay > Alike > Unifast TRAD > Luxatemp Plus, Protemp 3 Garant, Luxatemp Fluorescence. The mean heat capacity was 287.2 J/g (+/- 107.68). The heat capacity of the polymer-based provisional materials decreased in the following order: Duralay > TRAD, Jet, Alike > Snap, Luxatemp Fluorescence, Protemp 3 Garant, Luxatemp Plus. CONCLUSION: The heat capacity of materials, determined by D.S.C., is a factor in determining the thermal insulating properties of restorative materials. The peak temperature of PMMA was significantly higher than others (PEMA, dimethacrylate). No significant differences were found among PEMA (Snap) and dimethacrylate (P > 0.05). The time to reach peak temperature was greatest with PEMA, followed by PMMA and dimethacrylate. The heat capacity of PMMA was significantly higher than others (PEMA, dimethacrylate). No significant differences were found among PEMA and dimethacrylate (P>0.05).
Calorimetry, Differential Scanning*
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Crowns*
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Denture, Partial, Fixed*
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Fluorescence
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Hot Temperature
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Polymerization
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Polymers
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Polymethyl Methacrylate
10.Preparation and characterization of solid dispersions of ginkgolides.
Linyi MA ; Limei HAN ; Zhirong ZHANG ; Jianxin WANG
China Journal of Chinese Materia Medica 2009;34(11):1368-1372
OBJECTIVETo optimize the preparation process of solid dispersions of ginkgolides to improve the drug dissolution.
METHODThe influence of formulation and preparation technology on drug release from solid dispersions was investigated by single factor test. The X-ray diffraction analysis (XRD) and differential scanning calorimetry (DSC) were used to characterize the solid dispersions of ginkgolides.
RESULTThe solubilization efficiency of solid dispersions using PVP k30 as carrier was better than that taking poloxamer 188 or HPMC as matrix. The results of XRD and DSC showed that ginkgolides existed in solid dispersion at amorphous form or solvates form. The dissolution rate of ginkgolide B in solid dispersion was increased dramatically compared with raw material.
CONCLUSIONSolid dispersions could significantly improve solubility and dissolution rate of ginkgolides.
Calorimetry, Differential Scanning ; Ginkgolides ; chemistry ; Pharmaceutical Preparations ; chemistry ; Solubility ; X-Ray Diffraction