Preservation of phenolic compounds on dried leaf infusion of Bauhinia forficata Link

Abstract Bauhinia forficata Link aqueous extract is usually recommended as a phytomedicine to reduce blood glucose levels and its biological activity has been linked to the presence of phenolic compounds from B. forficata preparations. Several drying processes are used in the production of dry herbal extracts, which may influence the chemical composition and efficacy of final herbal medicines. Due to significant chemical changes, defining appropriate drying processes is essential for phytopharmaceutical drug development. In view of this, we analyzed dried B. forficata leaf infusion (BFLI) extracts by HPLC-UV-MSn, followed by molecular networking analysis to evaluate the chemical profiles from dried extracts yielded by freeze-and spray-drying processes. The main metabolites detected included 11 ferulic/isoferulic acid derivatives and 13 glycosylated flavonoids. The qualitative chemical profiles were alike for both drying processes, whereas the relative abundance of some flavonoids was higher using spray-drying. Taken together, our results showed that freeze-and spray-drying preserved the phenolic profile of BFLI and suggested that spray-drying may be the most suitable to obtain its dried products. Along with studying the chemical profiles of dried herbal extracts, evaluating the influence of drying processes on the quality and chemical profiles of final products is pivotal and may benefit future research.

Spray dried extract of Calophyllum brasiliense Cambés produces a potent hypoglycemic effect and improves total serum cholesterol and triglycerides in diabetic rats / El extracto secado por pulverización de Calophyllum brasiliense cambés produce un potente efecto hipoglucémico y mejora el colesterol sérico total y los triglicéridos en ratas diabéticas / O extrato seco por aspersão de Calophyllum brasiliense Cambés produz um potente efeito hipoglicemiante e melhora o colesterol total e triglicérideos em ratos diabéticos

SUMMARY Introduction: The species Calophyllum brasiliense Cambés (Calophyllaceae) is widespread throughout Central and South America. The stem bark infusion is used for lowering blood glucose. Aim: To optimize the spray dry extract ofthis plant using a D-optimal experimental design. Materials and methods: As factors were used the air-drying speed (3.5-4.5 m3/h), the feed flow rate of the suspension (5-11 mL/ min), and the inlet air temperature (90-130 °C). The dried extract was characterized by measuring the phenolics and flavonoids content, moisture, the water activity, apparent densities, flowability, and compressibility. The antioxidant activity, the inhibitory activity of lipase and alpha-glycosidase, and the antiglycant activity of the spray dried extract (SDE) were evaluated. Subsequently, the hypoglycemic activity was evaluated in rats by monitoring the blood glucose level, triglycerides, and cholesterol. Results: Inlet air temperature and feed flow rate were the factors that most affected the yield and phenolic content. SDE showed a potent antioxidant effect (IC50 1.83 μg/mL), a potent a-glycosidase (IC50 74.45 μg/mL) and pancreatic lipase (IC50 27.33 μg/mL) inhibition. A potent antiglycation effect (IC50 9.45^g/mL) was also observed. Conclusion: the SDE showed a potent hypoglycemic effect at 100 mg/kg. These results suggest that SDE could activate four important pathways that can contribute to diabetes control.

Resumen Introducción: la especie Calophyllum brasiliense (Calophyllaceae) está muy extendida en Centro y Suramérica. La infusión del tronco reduce los niveles de glucosa en sangre. bjetivo: optimizar el extracto seco por aspersión (SDE) de esta planta utilizando un diseño experimental D-óptimal. Materiales y métodos: como factores se utilizaron la velocidad del gas secante (aire, 3,5-4,5 m3/h), la temperatura de entrada del aire fue 90-130 °C y la velocidad de alimentación, 5-11 mL/min. Se determinó el contenido de fenoles y flavonoides en el extracto seco, la humedad residual, la actividad del agua, las densidades aparentes, fluidez y compresibilidad. Se evaluó la actividad antioxidante e inhibidora de lipasa y alfa-glicosidasa y la actividad antiglicante. También se evaluó la actividad hipoglicemiante midiendo glucosa en sangre, triglicéridos y colesterol. Resultados: la temperatura del aire de entrada y la velocidad de alimentación afectaron, significativamente, el rendimiento y contenido de fenoles. El SDE mostró un potente efecto antioxidante (IC50 1,83 μg/mL), una potente inhibición de a-glicosidasa (IC50 74,45 μg/mL) y de lipasa pancreática (IC50 27,33 μg/ mL). Se observó un fuerte efecto antiglicante (IC50 9,45 μg/mL). Conclusiones: el SDE mostró un potente efecto hipoglicemiante a 100 mg/kg. Estos resultados sugieren que el SDE podría actuar activando cuatro vías importantes para el control de la diabetes.

RESUMO Introdução: a espécie Calophyllum brasiliense (Calophyllaceae) é amplamente distribuída na América do Sul e Central. A infusão da casca do caule reduz os níveis de glicose no sangue. Objetivo: otimizar o extrato seco por pulverização (SDE) desta planta usando um planejamento experimental D-ótimo. Materiais e métodos: a velocidade do gás de secagem ar (3,5-4,5 m3/h), a temperatura de entrada do ar (90-130 °C) e a taxa de alimentação (5-11 mL/min) foram usados como fatores. Foi determinado o teor de fenóis e flavonóides no extrato seco, a umidade residual, a atividade de água, as densidades aparentes, a fluidez e a compressibilidade. Avaliou-se a atividade antioxidante e a atividade inibitória de lipase e alfa-glicosidase, e a atividade antiglicante do extrato seco. A atividade hipoglicêmica foi avaliada em ratos diabeticos, medindo a glicose no sangue, triglicerídeos e colesterol. Resultados: a temperatura de entrada do ar e a taxa de alimentação afetaram significativamente o desempenho e o conteúdo de fenois. O SDE mostrou um potente efeito antioxidante (IC50 1,83 μg/mL), uma significativa inibição de a-glicosidase (IC50 74,45 ig/mL) e da lipase pancreática (IC50 27,33 μg/mL). Um forte efeito antiglicante também foi observado (IC50 9,45 μg/mL). O SDE mostrou um forte efeito hipogli-cemiente à concentração de 100 mg/kg. Conclusões: Esses resultados sugerem que o SDE poderia atuar ativando quatro vias importantes para o controle do diabetes.

Establishment of online quantitative model for moisture content determination of hydroxychloroquine sulfate particles by near infrared spectroscopy / 药学实践杂志

Objective To establish an online quantitative analysis model for moisture content assay of hydroxychloroquine sulfate particles by near infrared (NIR) spectroscopy. Methods The NIR spectra were collected in real time when the material particles were dried in the fluidized bed. Meanwhile the water content of the particles was measured with the standard moisture tester. The multiplicative signal correction (MSC) and first derivative followed by Karl Norris smoothing were used for spectra pretreatment. Two spectral range (4 935−5 336 cm−1 and 6 911−7 297 cm−1) were selected for the quantitative model with the partial least squares (PLS) regression. Results The quantitative calibration model had good correlation coefficients with Rc value=0.952 9 and Rp value=0.936 6. The root mean square error of calibration (RMSEC) was 0.408 and the root mean square error of prediction error (RMSEP) was 0.435. The ratio of standard deviation of validation set to prediction standard deviation (RPD) was 5.18. There was no significant difference between the predicted value and the reference value by t test when the established model was applied in large-scale production. Conclusion The online model established for monitoring water content has high accuracy and stability, which can be applied in industrial scale process to monitor the particle moisture in real time.

Analysis on relativity of drying process of extract and pelleting quality of Chinese materia medica formula granule based on powder properties / 中草药

Chinese materia medica (CMM) formula granule is made from CMM extract powder and suitable pharmaceutical excipients, powder properties of CMM extract powder such as the particle size, hydroscopicity, and fluidity directly affect thepelleting quality of CMM formula granule. Drying is one of the indispensable operating units for preparations of CMM extract, which has great influence on the powder properties of CMM extract powder. Therefore, there is a certain correlation between the drying process and pelleting quality of CMM formula granule. Through the literature research, this paper summarizes the engineering principle and characteristics of each main granulation method, analysis of the evaluation factors of pellet quality, and combines with experimental research to explore the correlation between the drying process of CMM extract and pelleting quality of CMM formula granule in the perspective of powder properties. Finally, we puts forward that more attention should be payed to study the drying process of CMM extract, in order to further improve the quality of pelleting quality of CMM formula granule.

Initial study on preparation and properties of porous Bletilla striata polysaccharides gum / 中草药

Obiective Guided by the thought of unification of drug and adjuvant, Bletilla striata polysaccharides gum (BSPG) was got from traditional Chinese medicine of Bletilla striata. Methods In this research, the porous BSPG was prepared and its functional properties in solid and gel states were characterized by using infrared-assisted extraction, ethanol fractionation precipitation, freeze drying, and texture analyzer. BSPG40, BSPG60, and BSPG80 were fractionated by repeated precipitation method, using 40%, 60%,and 80% ethyl alcohol as precipitant and these polysaccharides content were determined with Phenylhydrate-Sulfuric acid. Octadecanol as the adjunct and the porous BSPG as the material, porous and non-porous tablets were prepared by direct compression method. The capabilities of floating, water absorption, expansibility, and the degradation performance were measured in artificial gastric juice to give an initial research on the feasibility that the porous BSPG can be used as adjuvant. Results It showed that the total polysaccharide content of BSPG, BSPG40, BSPG60, and BSPG80 was 64.15%, 69.33%, 57.64%, and 42.83%, respectively and the yield of BSPG40, BSPG60 and BSPG80 account for 83.25%, 12.16%, and 4.49%. BSPG80 is too little to get and exhibits typical “weak gel” properties, so properties of BSPG, BSPG40, BSPG60 were tested. By freeze drying, all samples were loose and porous. Hardness increased as the concentrations increased, and at equal concentrations, the hardness of BSPG, BSPG40, and BSPG60 gradually increased but filling power gradually decreased as the hardness increased. Elasticity of BSPG, BSPG40, and BSPG60 is better at the concentration of 15, 20, and 20 mg/mL respectively. While gel strength and adhesion of BSPG, BSPG40, and BSPG60 was gradually weaken. This study’s preliminary experiments indicated that tablets of porous BSPG had good ability of floating, water absorption, expansibility and the degradation performance. Conclusion The experiment results showed that different concentration of ethanol fractionation precipitation exercises a great influence on the texture properties and at the same time, different concentration of BSPG which obtained by the same concentration of ethanol fractionation precipitated has different texture properties and low concentrations of ethanol fractionation precipitated had better performance of hardness, filling power, gel strength, adhesion and played a better role in pharmacy. Besides, porous BSPG is a potential excipient of floating to prolong the gastric retention time. Therefore, this study provided important theoretical evidence and made great significance to future exploration and development of the new excipient of porous BSPG.

Influência do processo de secagem e condição de armazenamento de extratos secos de Bauhinia forficata e Passiflora alata sobre seu perfil de dissolução / Influence of the drying process and storage condition on the dissolution behavior of dried extracts of Bauhinia forficata and Passiflora alata

No Brasil, os produtos fitoterápicos são considerados medicamentos, sendo necessário o estabelecimento de estudos que assegurem a manutenção dos requisitos de qualidade durante o processamento e o armazenamento. Testes de dissolução podem ser empregados para se estimar a biodisponibilidade de um fármaco, sendo uma análise rotineira no desenvolvimento e controle de qualidade de medicamentos alopáticos. A determinação do perfil de dissolução de fitoterápicos também pode ser um importante critério para avaliação da sua qualidade lote-a-lote, bem como para os estudos de desenvolvimento e de estabilidade. O objetivo deste trabalho foi investigar a influência dos métodos de secagem e da condição de armazenagem sobre os perfis de dissolução dos flavonoides totais de extratos secos de duas plantas medicinais bastante difundidas no Brasil, a Bauhinia forficata e a Passiflora alata. Os extratos secos foram produzidos pelo processo de secagem em leito de jorro e em spray drying, sendo submetidos a condições de armazenagem aceleradas (temperatura de 40 ± 2ºC e umidade relativa de 75 ± 5%, por um período de 90 dias). Os perfis de dissolução foram obtidos para amostras de extratos secos antes e após o período de armazenamento. O teor de flavonoides totais foi quantificado por espectrofotometria. Os extratos secos de B. forficata e P. alata apresentaram adequada liberação de flavonoides nos ensaios de dissolução. Os extratos secos de Passiflora alata apresentaram completa dissolução dos flavonoides, 92% e 98% dos teores originais após 60 minutos de ensaio, respectivamente para o extrato seco em leito de jorro e em spray drying.

In Brazil, most of the herbal medicinal products are considered as medicine. Therefore, it is necessary the establishment of tests to guarantee the maintenance of quality requirements during their processing and storage. The dissolution test is used to estimate the bioavailability of drugs and is routinely used in the development and the quality control of allopathic medicines. The determination of the dissolution profile of herbal products can also be an important criterion for assessing the batch-to-batch quality as well as for studies of product development and stability. This work aimed to investigate the dissolution profiles of dried extracts of two medicinal plants widely used in Brazil, the Bauhinia forficata and Passiflora alata, by assessing the effect of the drying methods and storage condition on the release of the total flavonoid contents. Spouted bed and spray drying were the processes used for the production of the dried extracts. The products were subjected to accelerated storage conditions (temperature of 40 ± 2ºC and relative humidity of 75 ± 5%, for 90 days). The dissolution profiles of the dried extracts, before and after storage, were determined. The concentration of total flavonoids was quantified by spectrophotometry. Adequate dissolution profiles of flavonoids from B. forficata and P. alata were obtained for all the dried extracts produced. The dried extracts of Passiflora alata showed the complete dissolution of flavonoids in the dissolution media investigated, respectively 92% and 98% of flavonoids present in the dried extracts in spouted bed and spray drying after 60 minutes of the dissolution testing.

Content change of active components of yinqiao analogus preparations in different preparation processes / 中国药学杂志

OBJECTIVE: To investigate the key factors in the preparation process of yinqiao analogus preparations by comparing the contents of active ingredients after different preparation processes. METHODS: HPLC was employed to determine the contents of the active ingredients, and the changes of the active ingredients in the extracting-concentrating-drying process chain were investigated. Analytic hierarchy process (AHP) was used to determine the weighted coefficient for comprehensive evaluation of the multiple ingredients for different preparations. RESULTS: The highest loss rate of active ingredients occurred in the concentrating-drying process. The contents of the active ingredients in soft capsules and tablets were similar in the extraction, concentration and drying processes and all higher than those of the granules. The loss rates of chlorogenic acid, liquiritin, glycyrrhiz-in, and forsythoside A were higher than other ingredients in the whole process. In the AHP evaluation, yinqiaojiedu soft capsules got the highest score, followed by yinqiaojiedu tablets and yinqiaojiedu granules. CONCLUSION: The concentrating-drying process is the key process of yinqiao analogus preparations. Among the three preparation process, the highest retention rate of chlorogenic acid is yinqiaojiedu tablets process. However, results of AHP evaluation for other active ingredients show that yinqiaojiedu soft capsules processing would be better than the other two.

"Sweating" of traditional Chinese medicinal materials during primary processing and its mechanisms of enzymatic reaction and chemical conversion / 中草药

Primary processing of traditional Chinese medicinal materials (TCMM) is an important link which closely relates to the quality of products in TCMM. The traditional primary processing method and technology systems were derived from the long-term practices and experiences, which are distinctive, colorful, diverse, and scientific. The method of "sweating" is a critical step for processing the rhizome, root, cortex, and sclerotium and helpful for distributing moisture from inside to outside of TCMM in drying process, regulating and promoting the enzymatic reaction and chemical conversion by enzyme and germs, and starting or accelerating the biotransformation and chemical conversion of primary/secondary metabolites, which could directly affect the quality of TCMM. In this paper, the authors discuss the origins and development, purpose, and significance of "sweating" processing and the mechanisms of enzymatic reaction and chemical conversion of chemical compositions during the primary processing of "sweating". These data may provide the foundation and support for processing in normalization and standardization and formulating the Standard Operating Procedure (SOP) of primary processing of TCMM.

Effect of different drying and storing methods on quality control for leaves of Eucommia ulmoides / 中草药

Objective: To study the effect of different drying and storing methods on the content of main components in the leaves of Eucommia ulmoides. Methods: The contents of chlorogenic acid, geniposide acid, and geniposide in the leaves of E. ulmoides after being treated with different drying and storing methods were determined by HPLC. Results: The contents of geniposide acid and geniposide were higher in the fresh leaves of E. ulmoides and the content of chlorogenic acid was higher in the shade dried leaves of E. ulmoides after dried, microwave heated, and stored under low temperature. The content of main components in the leaves of E. ulmoides stored in darkness at low temperature decreased slowly. Conclusion: The contents of main components in the leaves of E. ulmoides collected in the best harvest time remain almost the same after fixed, dried, microwave heated, sealed, stored at low temperature in darkness for one year.

Influência dos processos de secagem sobre o teor de flavonoides e na atividade antioxidante dos extratos de Baccharis articulata (Lam.) Pers., Asteraceae / The Influence of drying processes on flavonoid level and the antioxidant activity of Baccharis articulata (Lam.) extracts

O objetivo deste trabalho foi verificar o teor de quercetina obtido dos extratos de partes aéreas de Baccharis articulata (Lam.) Pers., Asteraceae, submetidas a diferentes técnicas de secagem, bem como a avaliação de sua atividade antioxidante in vitro. Foi verificada maior concentração deste flavonoide nas amostras secas em estufa, porém não houve diferença significativa na atividade farmacológica das amostras analisadas.

The objective of this work was to verify the influence of different drying processes on the levels of quercetin of the aerial parts of Baccharis articulata (Lam.) Pers., Asteraceae, as well as the evaluation of the in vitro antioxidant activity of these extracts. We demonstrated that the highest concentration of this flavonoid was detected in oven-dried samples, although there no significant difference in their pharmacological activity of all analyzed samples could be shown.

Determining the potency of measles vaccine using plaque method

Background: Measles vaccine was the only vaccine in the expanded vaccination program still must be imported. Center for research and production of vaccines and biologicals \ufffd?Ha Noi was conducting the first stages of measles vaccine manufacturing technology transfer from the Kitasato Institute in Japan. The Center received semi-finished vaccine to set up finished vaccine production process as well as the testing process. Potency test and its consistency is very essential in quality control. Objectives: In order to identify standard potency assessment methods and potency of 13 lots of finished measles vaccine produced in Viet Nam from imported semi-finished products. Subjects and method: 13 lots of the finished vaccine were determined potency by plaque method based on 13 samples of semi-finished vaccine and the standard sample M16-6 had potency from 4.2 to 4.6 lg PFU/0.5 ml provided by the Kitasato Institute. Results: The result of 13 lots show that the reduction of potency during freeze-drying is within the range (0-0.76 lg); and 4 last consecutive lots are met WHO criteria on heat stability. Conclusion: This shows that the measles vaccine freeze-drying process in Vietnam was officially set up to use for the measles vaccine production in 2007.

Research into the standard process of fresh freeze - dried plasma for providing medical treatments with dutch dryer LY3-TTE/DM8

Background: Freeze - Dried Plasma (FDP) has many advantages, which could be stored for a long \ufffd?term and transported across remote areas for providing medical treatments and emergency aid. Objectives: To study the standard process of freeze - dried fresh plasma. Subjects and methods: 10 samples of fresh plasma from volunteer donors were selected according to certain categories. Plasma samples were frozen at \ufffd?75oC in 12 hours, freeze - dried at - 45oC and at the atmospheric pressure of 0.04mbar with Dutch dryer Ly - TTE/DM8. The adequate freeze - drying time for every 100ml of plasma was 60 hours. The protein level, factor VIII, electrolysis, the pH of plasma before and after the drying process were evaluated. Results: Results of tracking protein level in comparison between before and after freeze - dry showed the components and levels of freeze-dried protein changed little, with no statistical significance (P>0.05). The clotting factor before and after freeze-dried retains standard activity. After the freeze-dried process, factor VIII achieved 0.80 Ul/ml, prothombin achieved >80%. However, prothrombin decreased clearly (P<0.05). Electrolytes and pH changed had no statistical significance (P> 0.05). Conclusions: The procedures are applicable for processing and manufacturing drying plasma for long-term-storage and medical treatment. \r\n', u'\r\n', u'\r\n', u'

Preparation and Quality Evaluation of Lisinopril Polyvinyl Alcohol Particles / 中国药房

OBJECTIVE:To prepare lisinopril-loaded polyvinyl alcohol(PVA)particles(LIS-PVA-P)and establish its quality control method. METHODS:LIS-PVA-P was prepared by spray-drying process with PVA as carrier. The preparation was detected in terms of morphology,particle size,span,drug-loading capacity,encapsulation and in vitro dissolution. RESULTS:The preparation assumed sphere with porous surface. The average particle size was 17.29 ?m while drug-loading capacity 31.40%,encapsulation 94.20%,Span was 0.88,90% of the drug loads were released within 30 min. CONCLUSION:The preparation process is simple,good in repeatability and qualified in quality.

Study on drying process for Radix Tripterygii Wilfordii / 中成药

Objective: To determine the condition of drying process for Radix Tripterygii Wilfordii extract. Methods: Under different dying temperature and time, both triptolide and triptophenolide extracted from extract of Radix Tripterygii Wilfordii were measured. Results: After Radix Tripterygii Wilfordi extract was dried for 48 hours at 80 ?C , loss of triptophenolide and triptolide was relatively low, but after dried more than 48 hours at 100 ?C , the content of triptophenolide and triptolide reduced by 15.0%～30.0%. Conclusion: Drying temperature for Radix Tripteryqii Wilfordii extract should be controlled under 80 ?C .