Assessing compatibility of excipients selected for a sustained release formulation of bilberry leaf extract

Abstract The study is aimed to assess the compatibility of bilberry leaf powder extract (BLPE) with six excipients selected for sustained-release (SR) tablet formulation. The BLPE was obtained with the addition of L-arginine and Myo-inositol as the carriers. Thermogravimetric (TG-DTG) analysis and Fourier-transform infrared spectroscopy (FTIR), supported by Pearson correlation analysis, were applied to detect possible interactions in the binary mixtures (1:1) of the BLPE with each excipient. The TG-DTG showed some deviations in the thermal behavior of the BLPE / excipient mixtures. However, only the thermal behavior of magnesium stearate in the mixture significantly differed from individual samples, which suggested chemical interaction for this excipient. The FTIR analysis confirmed that the BLPE is compatible with Eudragit L100, Methocel K4M, Methocel K100LV, Avicel PH-101, and Plasdone S-630. Whereas it undergoes solid-state chemical interaction in the binary mixture with magnesium stearate. According to the FTIR-spectra, it is suggested that this interaction results in the formation of stearic acid and alkalization of the medium. These findings evidence for the possibility of using TG-DTG analysis as an independent thermal technique for compatibility studies and also confirm the earlier reported interaction of basic lubricants, e.g., stearic salts, with active ingredients containing amino groups.

Thermo-kinetics of Forest Waste Using Model-Free Methods / Termocinética de residuos de bosque usando los métodos de modelo libre / Termocinética de resíduos de bosque usando métodos de modelo livre

Abstract Thermal behaviour of pine needles (Pinus Roxburghii) is examined through a thermogravimetry technique. The dried samples of pine needles undergo the non-isothermal decomposition at temperature range of 308-1173 K. The heating rates used for experimental purposes are: 5 ◦ C min-1, 10 ◦ C min-1 and 15 ◦ C min-1. Kinetic parameters of thermal decomposition reactions of pine needles are obtained through the model-free schemes. The estimated values of activation energy and frequency factor derived from Kissinger method are 132.77 kJ mol-1 and 13.15 x 107 min-1, respectively. Furthermore, the averaged values of the same kinetics parameters retrieved from the isoconversional methods are 82.38 kJ mol-1 and 74.833 kJ mol-1, 25.42 x 1013 min-1 and 13.449 x 1010 min-1, respectively. Instead of the Flynn-Wall- Ozawa (FWO) and Kissinger- Akahira- Sunrose (KAS) schemes, the kinetic parameters derived from the Kissinger method are relatively promising for the thermal decomposition process, since the kinetic parameters are highly affected by intermediate stages and overlapping of the concurrent reaction occurred during pyrolysis.

Resumen Se examina el comportamiento térmico de las agujas de pino (Pinus roxburghii) a través de la técnica de termogravimetría. Las muestras secas de las agujas de pino se someten a una descomposición no isotérmica en un rango de temperatura de 308-1173 K. Las tasas de calentamiento usadas para los propósitos experimentales son: 5 °C min-1, 10 °C min-1 y 15 °C min-1. Los parámetros cinéticos de las reacciones de descomposición térmica de las agujas de pino se obtuvieron a través de esquemas de modelo libre. Los valores estimados de la energía de activación y el factor de frecuencia derivado del método Kissinger son: 132.77 kJ mol-1 y 13.15 x 107 min-1, respectivamente. Por otra parte, los valores promediados de los mismos parámetros cinéticos recuperados por los métodos isoconversionales son 82.38 kJ mol-1 y 74.833 kJ mol-1, 25.42 x 1013 min-1 y 13.449 x 1010 min-1, respectivamente. A diferencia de los esquemas Flynn-Wall-Ozawa (FWO) y Kissinger-Akahira-Sunrose (KAS), los parámetros cinéticos derivados del método Kissinger son relativamente promisorios para los procesos de descomposición térmica, ya que estos parámetros se afectan grandemente por los estados intermedios y la superposición de la reacción concurrente que ocurre durante la pirólisis.

Resumo O comportamento térmico de agulhas de pinheiro (Pinus roxburghii) foi examinado por meio da técnica de gravimetria. As amostras secas das agulhas de pinheiro se submeteram a uma decomposição não-isotérmica em uma faixa de temperatura de 308-1173 K. As taxas de aquecimento usadas para propósitos experimentais foram: 5 °C min-1, 10 °C min-1 e 15 °C min-1. Os parâmetros cinéticos das reações de decomposição térmica das agulhas de pinheiro se obtiveram por meio de esquemas de modelo livre. Os valores estimados da energia de ativação e o fator de frequência derivado do método Kissinger são: 132.77 kJ mol-1 e 13.15 x 107 min-1, respectivamente. Adicionalmente, os valores médios dos mesmos parâmetros cinéticos recuperados pelos métodos isoconversionais são 82.38 kJ mol-1 e 74.833 kJ mol-1, 25.42 x 1013 min-1 y 13.449 x 1010 min-1, respectivamente. Diferentemente dos esquemas Flynn-Wall-Ozawa (FWO) e Kissinger-Akahira-Sunrose (KAS), os parâmetros cine'ticos derivados do método Kissinger são relativamente promissórios para os processos de decomposição térmica, já que estes parâmetros são altamente afetados pelos estados intermediários e sobreposição da reação concorrente que ocorre durante a pirólise.

Hygroscopicity Study of Vitamin B12 Chemical Reference Substance / 中国药学杂志

OBJECTIVE: To investigate the hygroscopicity of vitamin B12 and the related problems of its chemical reference substance (CRS) that should be paid attention to. METHODS: UV absorption coefficient was determined at 361 nm, using water as solvent. Dynamic vapor absorption analysis (DVS) was applied to evaluate the moisture sorption trend and capacities of vitamin B12 under different humilities. RESULTS: Owing to the strong hygroscopicity of vitamin B12, deviation in the process of weighing might result in smaller UV absorption coefficient compared with the actual value, especially for dried and low moisture content raw materials in high-humidity environment. CONCLUSION: In the study of drug quality control for vitamin B12, the strong hygroscopicity of the raw material should be paid attention to, particularly in the research and application of vitamin B12 CRS.

Efficient immobilization of agarase using carboxyl-functionalized magnetic nanoparticles as support

Background: A simple and efficient strategy for agarase immobilization was developed with carboxyl-functionalized magnetic nanoparticles (CMNPs) as support. The CMNPs and immobilized agarase (agarase-CMNPs) were characterized by transmission electron microscopy, dynamic light scattering, vibrating sample magnetometry, scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, and zeta-potential analysis. The hydrolyzed products were separated and detected by ESI-TOF-MS. Results: The agarase-CMNPs exhibited a regular spherical shape with a mean diameter of 12 nm, whereas their average size in the aqueous solution was 43.7 nm as measured by dynamic light scattering. These results indicated that agarase-CMNPs had water swelling properties. Saturation magnetizations were 44 and 29 emu/g for the carriers and agarase-CMNPs, respectively. Thus, the particles had superparamagnetic characteristics, and agarase was successfully immobilized onto the supports. Agaro-oligosaccharides were prepared with agar as substrate using agarase-CMNPs as biocatalyst. The catalytic activity of agarase-CMNPs was unchanged after six reuses. The ESI-TOF mass spectrogram showed that the major products hydrolyzed by agarase-CMNPs after six recycle uses were neoagarotetraose, neoagarohexaose, and neoagarooctaose. Meanwhile, the end-products after 90 min of enzymatic treatment by agarase-CMNPs were neoagarobiose and neoagarotetraose. Conclusions: The enhanced agarase properties upon immobilization suggested that CMNPs can be effective carriers for agarase immobilization. Agarase-CMNPs can be remarkably used in developing systems for repeated batch production of agar-derived oligosaccharides.

A comparative study on different processes of inclusion of pericarpium citri reticulatae - Radix Aucklandiae essential oil preparation / 国际中医中药杂志

Objective To studyeffect of different processes for preparation ofβ- cyclodextrin inclusion pericarpium citri reticulatae - Radix Aucklandiae essential oil.Methods Extract pericarpium citri reticulatae-radix aucklandiae essential oil with steam distillation method, conductβ- cyclodextrin inclusion of pericarpium citri reticulatae-radix Aucklandiae essential oil with ultrasonic method, grinding method andsaturated aqueous solution method, and detect inclusion effect respectively by polarized light microscopy observation method and TG-DTA analysis method.Results Polarized lightphenomenon disappears under a microscope for the three inclusion preparation products, and TG-DTA curve of ultrasound method is superior to that of saturated aqueous solution method and grinding method.Conclusion Polarized light microscope observation method and TG-DTA method enjoysa good effect in determination of cyclodextrin inclusion, which provides a new method for determination of cyclodextrin inclusion results.

Evaluación de citrato de calcio y magnesio obtenido de dolomitas cubanas / Evaluation of calcium and magnesium citrate from Cuban dolomite

INTRODUCTION: calcium and magnesium salts are used as nutritional supplements obtained from natural sources such as dolomite, which is a double complex of calcium and magnesium carbonate. In search of a calcium raw material with greater bioavailability, a process of obtaining calcium and magnesium citrate salt from dolomite deposits was developed. OBJECTIVE: to evaluate calcium and magnesium citrate from dolomite. METHODS: chemical and technological analysis, Powder X-ray Diffractometry attenuated total reflection-Fourier transform infrared spectrometry (ATR-FTIR), differential scanning calorimetry and thermogravimetric analysis were all used. RESULTS: the chemical analysis confirmed the existence of calcium (over 10 percent), and of magnesium (4.5 and 5 percent) whereas citric acid content was under 3 percent, The levels of toxic metals were below the maximum allowable limits for pharmaceutical products. The density values were below those of the dolomite, with high porosity and flow deficit. The X-ray diffractomery indicated that dolomite was transformed into calcium and magnesium citrate salts whereas, the infrared spectra showed the presence of characteristic COO¯, -OH and -CH2 groups of citrates. The differential scanning calorimetry showed that salt had three endothermic peaks at 101.7 ºC, 167.1 ºC y 194.6 ºC and on the other hand, termogravimetry analysis confirmed that 30.9 percent of the total mass is lost at temperatures lower than 295 ºC..CONCLUSIONS: the presence of calcium and magnesium citrate salt is corroborated(AU)

INTRODUCCIÓN: las sales de calcio y magnesio son utilizadas como suplementos nutricionales y se obtienen a partir de fuentes naturales, dentro de las cuales se encuentra la dolomita, que es un complejo doble de carbonato de calcio y magnesio. En la búsqueda de una materia prima de calcio con mayor biodisponibilidad, ha sido desarrollado un proceso de obtención de sales de citrato de calcio y magnesio a partir de dolomitas. OBJETIVO: evaluar el citrato de calcio y magnesio obtenido a partir de dolomita. MÉTODOS: se emplearon métodos de análisis químicos y tecnológicos, difracción de rayos X, reflexión total atenuada en el infrarrojo medio con transformada de Fourier, calorimetría diferencial de barrido y análisis termogravimétrico. RESULTADOS: los resultados del análisis químico demostraron la presencia de calcio (superior al 10 por ciento) y magnesio (entre 4,5 y 5 por ciento), mientras que el contenido de ácido cítrico fue menor al 3 por ciento. Los niveles de metales tóxicos estaban por debajo de los límites máximos permisibles para productos farmacéuticos. Los valores de densidades fueron inferiores a las densidades de la dolomita, con la presencia de un elevado porcentaje de porosidad y deficiente flujo. El análisis por difracción de rayos X demostró que la dolomita fue transformada en sales de citrato de calcio y magnesio, mientras que los espectros infrarrojos mostraron que las principales absorciones se corresponden con las de los grupos COO¯, -OH y -CH2, características todas de citratos. Los estudios por calorimetría diferencial de barrido indicaron que la sal presentaba tres transiciones endotérmicas a 101,7 ºC, 167,1 ºC y 194,6 ºC, y el análisis termogravimétrico corroboró que a temperaturas menores de 295 ºC ocurre una pérdida de masa que representa el 30,9 por ciento de la masa total. CONCLUSIONES: se corrobora la presencia de sal de citrato de calcio y magnesio(AU)

Analysis and Comparison on Essential Oil of Rhizome Atractylodes Before and After Processing / 世界科学技术-中医药现代化

This study was aimed to analyze changes of content and quantity of essential oil of processing drugs of Rhizome Atractylodes and to achieve the impact of pyrolysis characteristics for using excipients, in order to offer evi-dences for further research and its processing technology. Steam distillation was used to extract essential oil in the Rhizome Atractylodes. Infrared spectroscopy and gas chromatography were used in the qualitative and quantitative analysis on constituents of essential oil of processing products of Rhizome Atractylodes. Thermogravimetric analysis was used in the comparison of pyrolysis characteristics between Rhizome Atractylodes and its excipients. The results showed that the content of essential oil was declined after processing. However, after being processed, the content of atractylodin was increased at different degrees compared to crude product. The change of atractylodin showed differ-ent tendency in different processing drugs. The atractylodin content from high to low was in the order of products stir-baked to yellowish, products roasted by bran, products prepared with rice water, crude drug. At the temperature of more than 220oC, excipients had major impact for the pyrolysis characteristics of Rhizome Atractylodes. It was concluded that the essential oil declined, but atractylodin increased after Rhizome Atractylodes being processed. It also provided experimental basis for further research on processing technology, ormulation of quality standard and improvement of processing mechanism.

The evaluation of coated granules to mask the bitter taste of dihydroartemisinin / A avaliação de grânulos revestidos para mascarar o sabor amargo da diidroartemisina

The purpose of this study was to mask the bitter taste imparted by dihydroartemisinin (DHA) by the use of different coating materials. Trial-1 and trial-2 were conducted to prepare the DHA granules. The granules produced from trial-1 were irregular in shape and smaller in size while the trial-2 granules were more regular and larger in size. The granules obtained from both trials were then coated with two different coating methods, namely A and B, depending upon coating material. The trial-2 granules showed better flow properties than trial-1 granules. In vitro dissolution studies in phosphate buffer at pH 6.8 revealed that granules of trial-2B released only 34 percent ± 3 DHA in two minutes compared with trial-1A (57 percent ± 2), trial-1B (48 percent ± 2) and trial-2A (53 percent ± 7). The pleasant taste perception (PTP) test also confirmed the taste masking efficacy of trial-2B (P < 0.05). Scanning electron microscopy (SEM) revealed the more regular and smooth surface of trial-2B granules. In addition, the differential thermal and thermogravimetric analysis (TG-DTA) confirmed no interaction between the materials and pure DHA. DHA has shown its characteristic peaks in the x-ray diffraction (XRD) patterns which were also prominent in all the granules. In conclusion, the granules obtained from trial-2B displayed considerable decrease in the bitter taste of DHA thereby fulfilling the purpose of this study.

O objetivo deste estudo foi o de mascarar o gosto amargo característico da diidroartemisinina (DHA) pelo uso de diferentes materiais de revestimento. Experimento-1 e experimento-2 foram realizados para preparar grânulos de DHA. Os grânulos produzidos pelo experimento-1 mostraram-se irregulares e menores se comparados aos obtidos pelo experimento-2, que foram mais regulares e maiores. Os grânulos obtidos em ambos os experimentos foram, então, revestidos por dois métodos distintos de revestimento, designados como A e B, dependendo do material de revestimento empregado. Os grânulos do experimento-2 mostraram melhor propriedade de fluxo que os obtidos no experimento-1. Estudos de dissolução in vitro em tampão fosfato pH 6,8 revelaram que grânulos do experimento-2B liberaram apenas 34 por cento ± 3 da DHA em dois minutos se comparado com experimento-1A (57 por cento ± 2), experimento-1B (48 por cento ± 2) e experimento-2A (53 por cento ± 7). A Análise Sensorial quanto ao sabor (Pleasant Taste Perception - PTP) também confirmou a eficácia do experimento-2B (P <0,05) em mascarar o gosto amargo da DHA. Microscopia Eletrônica de Varredura (SEM) revelou a superfície mais regular e lisa dos grânulos obtidos pelo experimento-2B. Além disso, Análise Termogravimétrica e Análise Térmica Diferencial (TG-DTA) confirmaram que não há nenhuma interação entre os materiais e a DHA pura. DHA mostrou seus picos característicos na Difração de Raios X (XRD) em padrões que também foram proeminentes em todas as amostras. Em conclusão, os grânulos obtidos pelo experimento-2B exibiram diminuição considerável no gosto amargo da DHA, o que era o propósito deste estudo.

Preparation and characterization of peppermint oil-β-cyclodextrin polymer microsphere inclusion compound / 中草药

Objective: To optimize the including preparation for peppermint oil-β-cyclodextrin polymer (β-CDP) microsphere inclusion compound. Methods: Peppermint oil-β-CDP microsphere inclusion compound was prepared by using co-precipitation. The preparation process was optimized through the L9(34) orthogonal test design and regression analysis. Peppermint oil-β-CDP microsphere inclusion compound was characterized by infrared (IR) spectroscopy, thermogravimetric analysis (TGA), and X-ray diffraction (XRD). Results: The best technological condition was A 2B2C1D3, and the order of the influence factors was the proportion of β-CDP microsphere and water > the percentage of peppermint oil in β-CDP microsphere > inclusion temperature > inclusion time. The formation of peppermint oil β-CDP microspheres inclusion compound was proved by the results of IR, XRD, TGA analyses. Conclusion The method is reasonable and feasible.

Análisis termogaavimétrico en la caracterizació de carbones Colombianos empleaados en la producción de coque / Themogravimetricc analysis in the characterization f Colombian coaals used in the production of coke / Análise termogrvvimétrica na caracterização de carvões Colombiaos utilizados nna produção de coque

Cinco carbones de los departamentos de Cundinamarca, Boyacá y Norte de Santander (Colombia) se caracterizaron mediante análisis próximo, último, reológico, petrográfico, calorífico y termogravimétrico. Los parámetros analizados, especialmente aquellos que determinan las propiedades reológicas, muestran que los carbones estudiados y sus mezclas podrían producir un coque de buena calidad. Se observó la relación inversa entre el contenido de materia volátil y la reflectancia media aleatoria de la vitrinita, que se atribuye al aumento de la aromaticidad en la estructura molecular del carbón como una consecuencia del incremento en el rango. Los parámetros derivados del análisis termogravimétrico -máxima velocidad de desvolatilización y temperatura de máxima velocidad de desvolatilización- mostraron buenas correlaciones con la reflectancia media aleatoria de la vitrinita, igual que la máxima velocidad de desvolatilización con la fluidez máxima. Lo anterior indica que el análisis termogravimétrico podría ser una herramienta útil para caracterizar de manera rápida carbones usados en procesos de fabricación de coque metalúrgico.

Five types of coal from the states of Cundinamarca, Boyaca and Norte de Santander (Colombia) were characterized by proximate, ultimate, rheological, petrographic, calorific and thermogravimetric analysis. The parameters used, especially the ones which determine the rheological properties show that the studied coals and its blends could produce good quality coke. It was observed the inverse relationship between the volatile matter content and the mean vitrinite reflectance, relationship which is attributed to the increase of the aromaticity in the molecular structure of the coal as a consequence of the rank increase. The parameters derived from the thermogravimetric analysis, maximum velocity of de-volatilization and the temperature of maximum velocity of de-volatilization and the media reflectance of the vitrinite showed good correlations. Also was observed an interesting correlation between the velocity ofde-volatilization and maximum fluidity. This shows that the thermogravimetric analysis can be a useful tool to characterize in a quick way coals used for metallurgical coke production.

Cinco carvões dos departamentos de Cundinamarca, Boyacá e Norte de Santander (Colômbia) foram caracterizados por análise próxima, última, reológica, petrográfica e termogravimétrica. Os parâmetros analisados, em especial aqueles que determinam as propriedades reológicas mostram que os carvões estudados e suas misturas podem produzir coque de boa qualidade. Foi observada relação inversa entre o teor de matéria volátil e refletância média vitrinite, que é atribuído ao aumento da aromaticidade da estrutura molecular do carvão como um resultado do aumento no rango. Os parâmetros derivados da análise termogravimétrica, velocidade máxima de pirólise e temperatura de máxima velocidade de pirólise mostraram boas correlações com a refletância média vitrinite, tal como a velocidade máxima de pirólise e a fluidez máxima. Isto mostra que a análise termogravimétrica pode ser uma ferramenta útil para caracterizar rapidamente carvões utilizados nos processos de fabricação de coque metalúrgico.

Dipteryx lacunifera seed oil: characterization and thermal stability / Óleo de sementes de fava de morcego: caracterização e estabilidade térmica

The Dipteryx lacunifera Ducke is an oleaginous legume with high oil and protein content that can be used in human nutrition. The specie is a native of the Piauí and Maranhão state in the north east of Brazil. The measure physico-chemical properties of the oil are specific density, refractive index, acid, peroxide, iodine and saponification values of 0.91, 1.4651, 0.60 ( percent oleic acid), 2.81, 70.80 and about 179, respectively. Gas chromatographic analysis of the oil showed the presence of 20.6 percent saturated, 65.1 percent monounsaturated and 14.3 percent polyunsaturated fatty acids. The saturated fatty acids C6:0, C8:0, C12:0 and C17:0 were present in trace (<0.01 percent) amounts while the C16:0, C18:0, C20:0, C22:0 and C24:0 were at concentrations of 10.3, 5.4, 3.4, 0.9 and 0.6 percent of the total fatty acids. Unsaturated fatty acids C18:1, C18:2, C18:3 and C22:2 contents were 65.1, 14.1, 0.3 percent and trace (0.01 percent), respectively. Thermal analysis (TG/DTG) revealed that the thermal decomposition of the oil occurs in two steps corresponding to the unsaturated and saturated fatty acids. The oil, when heated to a temperature of 180º C for 400 min showed smaller loss in mass than commercial soy, sunflower and corn oils. The curve DSC indicated an endothermic event with enthalpy variation (DH) of -56.7 Cal.g-1 in the temperature interval of 340 ºC (Ti) the 463º C (Tf), with maximum in 411.1º C (Tm).

A Dipteryx lacunifera Ducke (fava de morcego) é uma leguminosa oleaginosa com elevado conteúdo em proteínas e óleo podendo ser usada na nutrição humana. A espécie é nativa dos estados do Piauí e Maranhão do nordeste do Brasil. Mensurações das propriedades físico-químicas do óleo densidade especifica, índice de refração, acidez, peróxidos, iodo e saponificação foram 0.91, 1.4651, 0.60 ( por cento ácido oléico), 2.81, 70.80 e 179, respectivamente. A análise do óleo por cromatografia gasosa mostrou a presença de 20.6 por cento de ácidos graxos saturados, 65.1 por cento de monoinsaturados e 14.3 por cento poliinsaturados. Os ácidos graxos C6:0, C8:0, C12:0 e C17:0 estão presentes em quantidades de traços (<0.01 por cento) enquanto os C16:0, C18:0, C20:0, C22:0 e C24:0 estão em concentrações de 10.3, 5.4, 3.4, 0.9 e 0.6 por cento, respectivamente, dos ácidos graxos totais. O conteúdo dos ácidos graxos insaturados C18:1, C18:2, C18:3 e C22:2 foram 65.1, 14.1, 0.3 por cento e traço (0.01 por cento), respectivamente. A análise térmica (TG/DTG) revelou que a decomposição térmica do óleo ocorre em dois estágios correspondentes aos ácidos graxos insaturados e saturados. O óleo quando aquecido na temperatura de 180º C por 400 min mostrou menor perda massa que o óleo comercial de soja, girassol e milho. A curva DSC indicou um evento endotérmico com variação de entalpia (DH) de -56.7 Cal.g-¹ no intervalo de temperatura 340º C (Ti) a 463º C (Tf), com máximo em 411.1º C (Tm).

Análise térmica de uma resina composta de nanopartículas: caracterização e envelhecimento / Thermal analysis of nanofilled composite resin: characterization and aging

O objetivo deste estudo foi acompanhar o envelhecimento de uma resina composta de nanopartículas (Concept Advanced®) ao longo de um ano. A caracterização e a avaliação de sua homogeneidade foram realizadas após o envase em seringa de apresentação comercial por meio de Termogravimetria (TG/DTG), Calorimetria Exploratória Diferencial (DSC) e Análise Termomecânica (TMA). No grupo 1, foram realizadas 15 análises ao longo de seringas que não foram submetidas à pressão do êmbolo. Nos grupos 2 e 3, a resina composta foi totalmente removida pela torção do êmbolo e subdividida em cinco porções. Contudo, ao longo do tempo, no grupo 2, as seringas foram mantidas na vertical e no grupo 3, na horizontal. No grupo 4, cada amostra foi obtida de 24 em 24 horas da área central de cada porção por cinco dias. A análise dos diferentes grupos foi realizada em três seringas para os tempos: inicial, seis meses e um ano. As curvas TG/DTG foram obtidas em amostras não polimerizadas, seguindo programa de aquecimento de 25 a 650ºC, em atmosfera dinâmica de ar. A DSC e a TMA foram realizadas apenas no grupo 1, no tempo inicial, para caracterização do material em amostras fotoativadas de 3mm de diâmetro x 1mm de espessura por 20 segundos. As curvas DSC foram obtidas seguindo o programa de aquecimento da temperatura ambiente a 250°C, sob fluxo de nitrogênio. A TMA foi realizada em atmosfera de nitrogênio da temperatura ambiente a 150oC. As curvas TG/DTG de cada área analisada mostraram o mesmo padrão de decomposição em três etapas com percentuais de perda de massa semelhantes entre todas as amostras independente do tempo de armazenamento. Também o resíduo final, considerado como percentual de carga inorgânica, ficou em torno de 71,5% mostrando homogeneidade de distribuição ao longo das seringas. A pressão contínua determinou alteração estatisticamente significante na estabilidade térmica (p<0,05). Na DSC, as curvas mostraram temperatura de transição vítrea na faixa de 94 a 105ºC e um evento exotérmico a ~160ºC relacionado à polimerização secundária da resina composta. A TMA mostrou três faixas de alterações dimensionais e os valores do coeficiente de expansão térmica linear variaram dentro da mesma seringa, não mostrando homogeneidade de resultados.

The aim of this study was to evaluate the aging of a nanofilled composite resin (Concept Advanced®) during one year. The characterization and evaluation of its homogeneity in commercial syringe was made by Thermogravimetric Analysis (TG/DTG), Differential Scanning Calorimetry (DSC) and Thermomechanical Analysis (TMA). In group 1, 15 analyses throughout syringes were carried without pressing the pestle screw. In groups 2 and 3, the composite resin was all pressed out by the pestle screw and divided in five portions. However, in group 2, throughout the time, the syringes had been kept in the vertical position and group 3 in the horizontal position. In group 4, each sample was obtained every 24 in 24 hours from the central area of each portion during five days. All the analyses of groups 1, 2, 3 and 4 were carried through three syringes in the following times: initial, 6 months and one year. The TG/DTG analyses were carried in not polymerized samples, following a thermal program from 25 to 650ºC, under dynamic air atmosphere. The DSC and the TMA were just carried in group 1, in the initial time, to characterize the material in polymerized samples of 3mm diameter x 1mm thickness per 20 seconds. The curves DSC were obtained following the thermal program from room temperature to 250°C under a nitrogen flow. The TMA was carried under a nitrogen atmosphere from room temperature to 150°C. The curves of TG/DTG showed similar patterns of decomposition in three stages, in all groups independent of the storage time, with similar percentages of loss of mass. Also the weight fraction of inorganic fillers was around 71.5%, showing homogeneity of distribution throughout the syringes. The continuous pressure determined significant alteration in the thermal stability (p< 0,05). The DSC curves showed a glass transition ranged between 94 and 105ºC and eventually an exotherm event at ~160ºC. The TMA showed that the values of the linear coefficient of thermal expansion had varied inside of the same syringe

Thermal Stability and Thermal Decomposition Kinetics of Ciprofloxacin Hydrochloride / 中国药房

OBJECTIVE:To study the process and mechanism of thermal decomposition of ciprofloxacin hydrochloride(CPLX).METHODS:With Al2O3 as reference substance,the samples in nitrogen gas were analyzed by differential scanning calorimetry(DSC),thermogravimetry(TG),digital thermogravimetry(DTG).The thermal kinetic parameters including the energy of activation(E),pre-exponential factor(A),reaction order(n) and pk value were computed based on the data of the thermal analysis curves.RESULTS:The thermal kinetic parameters were as follows:E=101.18 kJ?mol-1,lnA=26.96 s-,n=1,and pk=7.01,and the storage life of ciprofloxacin hydrochloride under normal temperature was 2 years.CONCLUSION:The thermal analysis method is simple and the result is reliable in the study of thermal decomposition of ciprofloxa-cin hydrochloride.

Idendifications of Radix Ginseng and Radix Panacis Quinquefolii by Thermogravimetric Analysis / 中成药

The thermogravimetric analysis was developed for the identification of powders and extracts of Radix Ginseng and Radix Panacis Quinquefolii. This method is simple,quick and accurate with small sample. It is avaliable for the identification of true and false product series of Radix Ginseng and Radix Panacis Quinquefolii in current market.