Process optimization of physicochemical properties of spray-dried Hydrocotyle umbellata L. extract

Abstract Hydrocotyle umbellata L., Araliaceae, is a species that is recommended in Ayurvedic medicine for its effects on the central nervous system, such as anxiolytic and memory-stimulant effects. Despite the medicinal potential of this species, its phytopharmaceutical and technological potential to produce standardized extracts has not been investigated. This study analyzes the influence of spray drying parameters on the contents of the chemical markers (total phenolic, total flavonoid, and hibalactone) and the functional properties of H. umbellata extract. The optimization of drying conditions was performed using a central composite design combined with response surface methodology and desirability function approach. The mathematical models fitted to experimental data indicated that all the evaluated drying parameters significantly influenced the chemical contents. The optimal conditions were: inlet temperature of 120 °C, feed flow rate of 4 mL min-1, and colloidal silicon dioxide:maltodextrin ratio of 16%:4%. Under these conditions, the powder samples had spherical particles and desirable physicochemical and functional properties, such as low water activity and moisture content, good product recovery, reconstitution, and flowability. Thus, spray drying might be a promising technique for processing standardized H. umbellata extracts.

Cause Analysis and Solution Strategy of Poor Solubility of Dioscoreae Rhizoma Formula Granules / 中国实验方剂学杂志

Dioscoreae Rhizoma formula granules are made from decoction pieces by decocting， extracting， separating， concentrating， drying and granulating， which have the advantages of simple dispensing， convenient use and easy to take without decoction. However， because Dioscoreae Rhizoma is rich in starch and mucus components， its extract powder and formula granules are poorly soluble and difficult to dissolve or disperse completely within 5 min， and the insoluble material is difficult to dissolve completely even after 24 h in water， which affects the quality evaluation of the formula granules and medication psychology of patients. Therefore， by studying the dissolution process and mechanism of Dioscoreae Rhizoma extract and its formula granules， it was found that the special chemical composition of Dioscoreae Rhizoma， the denaturation of starch and its compounding with protein and other substances during the high temperature extraction process， and the contraction of coating membrane during the spray drying process were combined to form the special microstructure of coating membrane covering starch granules， and it is the root cause of poor solubility of Dioscoreae Rhizoma formula granules. Based on the research on the structure， property and function of the powder， this paper proposed a technical strategy to improve the solubility of Dioscoreae Rhizoma formula granules by powder modification process， and experimentally demonstrated that the modified Dioscoreae Rhizoma formula granules could completely dissolve within 2 min， which solved the technical problem and could provide reference for the improvement of solubility of other similar varieties， and promote the high-quality development of traditional Chinese medicine formula granule industry.

Spray-dried co-amorphous Tadalafil ternary mixtures: a promising platform towards the enhancement of solubility and bioavailability

Abstract Tadalafil (Tad) is a poorly water-soluble drug (BCS class II) that is used for the treatment of erectile dysfunction. An enhancement of aqueous solubility is vital to accelerate its onset of action and subsequently enhance its therapeutic effect. Binary and ternary mixtures of Tad with different amino acids (histidine, valine, alanine or arginine) and other excipients (mannitol and SLS) were prepared and then spray dried. The solubilizing efficiency and physicochemical characterization of all spray dried mixtures of Tad were studied. The optimum formulation was investigated in male rats to determine the onset of erection and the pharmacokinetic parameters of Tad. In general terms, the drug solubility of spray-dried formulae was enhanced compared to the crystalline form of the drug as a result of the formation of co-amorphous structures. The final result revealed that the Tad/alanine/mannitol spray-dried mixture (F10) showed the highest solubility and an improvement in its physicochemical characteristics. Moreover, F10 showed a significantly faster erection in rats with an improvement in Tad pharmacokinetic parameters when compared to the crystalline drug. Thus, F10 is selected as a promising formulation that successfully enhanced the bioavailability and the therapeutic efficacy of Tad.

Spray Drying in Research of Traditional Chinese Medicine Powders： A Review / 中国实验方剂学杂志

After more than 100 years of development， spray drying technology has become more mature and widely used， and it is of great importance in the field of traditional Chinese medicine （TCM）. TCM powders prepared by spray drying is the raw material of dispensing granules， and the powder properties have an important influence on subsequent molding process and product quality. As a new form of TCM， dispensing granules have been included in the management category of TCM decoction pieces， indicating a broader application market， and a consensus has also been reached on the importance of TCM powder research. Based on this， the author summarized the application progress of spray drying in the study of TCM powders， including the factors affecting spray drying process， such as liquid properties， process parameters and equipment factors， as well as the application of computational fluid dynamics （CFD） and thermodynamic model in spray drying process simulation. Moreover， some commonly used pharmaceutical excipients for the modification of TCM powders were also introduced such as maltodextrin， microcrystalline cellulose and povidone. In addition， spray drying technology can also be used as a preparation technology for new drug delivery systems such as microcapsules and solid dispersions. Through the summary of this paper， the author suggests that the future research direction of spray drying of TCM can be carried out from the aspects of application rule of the coprocessing auxiliary materials based on the "unification of medicines and excipients"， the "structure-property" relationship of spray-dried powders and the application of computer simulation and design， so as to further enrich the application of spray drying in the field of TCM powders.

Improvement on compactibility of the alcoholic extract of Zingiberis Rhizoma by co-spray drying with HPMC / 中国中药杂志

Aiming to solve the poor compactibility of the alcoholic extract of Zingiberis Rhizoma(ZR), this study explored the feasibility of its physical modification using co-spray drying with a small amount of hydroxypropyl methyl cellulose(HPMC). Based on the univariate analysis, the influence of two independent variables(the HPMC content in the product and the solid content of spray material) on the powder properties and tablet properties of the dried product was investigated by the central composite design. With the tensile strength and disintegration time of the tablets as the evaluation indexes, the optimal prescription was determined as follows: the HPMC content was 15% and the solid content of spray material was 25.6%. The accuracy of the regression model established for predicting tensile strength and disintegration time of tablets was verified, and the results revealed that the measured values were close to the predicted ones with deviations of 0.47% and-8.2%, indicating good prediction and reproducibility of the model. The tensile strength(4.24 MPa) of tablets prepared with the optimal prescription was 3.59 times that(1.18 MPa, far lower than the baseline of 2 MPa for qualified tablets) with the spray-dried powder of the ZR. On the other hand, due to the addition of HPMC, the disintegration time of tablets increased from 7.3 min to 24.6 min. On the whole, this study provided a new strategy to solve the common problem of poor compactibility of raw Chinese medicinal materials, which facilitated the successful preparation of Chinese medicinal tablets with high drug loads.

Effect of the drying method and texture improvers on reconstitution behavior of yogurt powder: physical and microbiological properties / Efecto del método de secado y mejoradores de textura sobre el comportamiento de reconstitución de un yogurt en polvo: propiedades físicas y microbiológicas

Background: One of the most used and effective preservation strategies in foods is drying. However, there are problems with the rheological properties, color, and viability of lactic acid bacteria in the yogurt once reconstituted when applying such conservation strategies. Objectives: Determine the concentration of the type of texture improver and drying that minimizes the negative effect on the rheological, color, and microbiological properties of a reconstituted yogurt powder. Methods: Intended to determine the texture improver which increases rheological properties of reconstituted yogurt powder, a mixture type experimental design was applied where three texture improvers were assessed; carboxymethylcellulose (CMC) (mass fraction 0 - 1), pectin (mass fraction 0 - 1), and xanthan gum (mass fraction 0 - 1). The rheological parameters; consistency index (K), flow behavior (n), viscosity at 100s-1 (η), the storage (G') and loss (G'') modules, and the phase shift angle (δ) of each of the reconstitutions were considered as design-dependent variables. Secondly, a central composite design (face-centered) was used for assessing the effectiveness of the drying (convection, spray-drying, and freeze-drying), the concentration of the texture improver (0.0 - 1.0 %), and the yogurt powder concentration (8.0 - 15.0 %). The above-mentioned rheological parameters, color, and viability of the lactic acid bacteria from each reconstituted yogurt powder were considered as the dependent variables. Optimization sought to match the parameters of reconstituted yogurt powder that approximated the conditions of fresh yogurt. Results: The independent variables in their lineal expression and some interactions between them had statistically significant differences (p < 0.05). At a concentration of 10.59 % with 0.03 % xanthan gum, the reconstitution of freeze-dried yogurt powder was the optimized condition (p < 0.05) and obtained the rheological, color, and microbiological parameters closest to fresh yogurt. Conclusions: The drying of the yogurt by freeze-drying mixed with xanthan gum as a texture improver allowed to obtain a reconstituted yogurt with properties close to the fresh product for direct consumption

Antecedentes: Una de las estrategias de conservación más utilizadas y efectivas en los alimentos es el secado. Sin embargo, existen problemas en las propiedades reológicas, el color y la viabilidad de bacterias ácido lácticas en el yogur una vez reconstituido al aplicar tales estrategias de conservación. Objetivos: Determinar la concentración del tipo de mejorador de textura y secado que minimiza el efecto negativo sobre las propiedades reológicas, de color y microbiológicas de un yogur en polvo reconstituido. Métodos: Para determinar el mejorador de textura que aumente las propiedades reológicas del yogur en polvo reconstituido, se aplicó un diseño experimental de tipo de mezcla donde se evaluaron tres mejoradores de textura; carboximetilcelulosa (CMC) (fracción de masa 0 -1), pectina (fracción de masa 0 -1) y goma xantan (fracción de masa 0 -1); los parámetros reológicos: índice de consistencia (K), comportamiento de flujo (n), viscosidad a 100s-1 (η), módulos de almacenamiento (G') y pérdida (G''), y ángulo de desfase (δ) de cada una de las reconstituciones fueron considerados como variables dependientes. En segundo lugar, se utilizó un diseño central compuesto (centrado a las caras) para evaluar el efecto del tipo de secado (convección, secado por aspersión y liofilización), la concentración del mejorador de textura (0.0 - 1.0 %) y concentración del yogur en polvo (8.0 - 15.0 %). Como variables dependientes se consideraron los parámetros reológicos mencionados anteriormente, el color y la viabilidad de las bacterias ácido lácticas de cada yogur en polvo reconstituido. La optimización buscó igualar los parámetros del yogur en polvo reconstituido que se aproximaran a las condiciones del yogur fresco. Resultados: Las variables independientes en su expresión lineal y algunas interacciones entre ellas tuvieron diferencias estadísticamente significativas (p < 0.05). La reconstitución de yogur liofilizado en polvo a una concentración de 10.59 % con 0.03 % de goma xantan, fueron las condiciones optimizadas (p < 0.05) que obtuvieron los parámetros reológicos, de color y microbiológicos más cercanos al yogur fresco. Conclusión: El secado del yogur por liofilización mezclado con goma xantan como mejorador de la textura, permitió obtener un yogur reconstituido con propiedades cercanas al producto fresco para consumo directo

Microencapsulación mediante secado por atomización a partir de un extracto de los cálices de Hibiscus sabdariffa L / Microencapsulation by spray drying from an extract of the calyces of Hibiscus sabdariffa L / Microencapsulação por secagem por pulverização a partir de um extrato dos cálices de Hibiscus sabdariffa L

Resumen La investigación tuvo como objetivo definir las mejores condiciones de extracción asistida por ultrasonido de los cálices de H. sabdariffa L. y la obtención de polvos microencapsulados, mediante secado por aspersión. Los extractos fueron analizados, considerando como variables: disolvente (agua y agua/etanol) y la relación temperatura/tiempo de extracción (25 °C/60 min y 60 °C/30 min). Para el secado se evaluaron las variables temperatura de entrada (150 °C; 190 °C) y la mezcla de encapsulantes goma arábiga (G) y maltodextrina (MD) (G40/ MD60; G60/MD40). Los parámetros utilizados para el análisis fueron: rendimiento, pH, °Bx, composición química (fenoles y antocianinas totales, CLAE-EM) y capacidad antioxidante (DPPH). La mejor condición para la extracción de polifenoles resultó ser con agua:etanol (80:20), a 60 °C y durante 30 min. Se identificó la presencia de ácidos fenólicos, glicósidos de flavonoles y las antocianinas (delfinidina-3-sambubiósido y cianidina-3-sambubiósido), como las señales de mayor intensidad. Con el secado por atomización a 150°Cy con G60/MD40, se logró el mayor contenido de fenoles totales y antocianinas, sin embargo, la capacidad antioxidante se favoreció a 150 °C y con G40/MD60. Las micropartículas obtenidas podrían valorarse como materia prima para la elaboración de fitofármacos o alimentos funcionales, considerando su fácil manipulación, posible estabilidad y su valor antioxidante.

Abstract The objective of the research was to define the best conditions for ultrasound-assisted extraction of H. sabdariffa L. calyces, and to obtain microencapsulated powders, by spray drying. The extracts were analyzed, considering as variables: extracting solvent (water and water/ethanol) and the temperature /extraction time ratio (25 °C/ 60 min and 60 °C/30 min). Inlet air temperature (150 °C; 190 °C) and the mixture of gum arabic (G) and maltodextrin (MD) as encapsulating agents (G40/MD60; G60/MD40) were the variables studied. The parameters used for the analysis were: yield, pH, °Bx, chemical composition (phenols and total anthocyanins, HPLC-MS), and antioxidant capacity (DPPH). The best polyphenols extraction conditions were water:ethanol (80:20), at 60 °C for 30 min. The presence of phenolic acids, flavonol glycosides, and anthocyanins (delphinidin-3-sambubioside and cyanidin-3-sambubioside) were identified as the signals of highest intensity. Inlet air temperature at 150 °C and G60/MD40 allowed the highest total phenols and anthocyanins content. However, the antioxidant capacity was better at 150 °C and G40/MD60. The microparticle obtained could be used as an ingredient for the preparation of phytopharmaceuticals or functional foods, considering their easy handling, and antioxidant capacity.

Resumo O objetivo da pesquisa foi definir as melhores condições para a extração assistida por ultrassom de H. sabdariffa L. calyces e obter pós microencapsulados, por meio de secagem por pulverização. Os extratos foram analisados considerando-se variáveis: menstruação (água e água/etanol) e a razão temperatura/tempo de extração (25 °C/60 min e 60°C/30 min). Para a secagem, os variais foram avaliados: temperatura de entrada (150 °C; 190 °C) e mistura dos encapsulantes goma arábica (G) e maltodextrina (MD) (G40/ MD60; G60/MD40). Os parâmetros utilizados para a análise foram: rendimento, pH, °Bx, composição química (fenóis e antocianinas totais, HPLC-MS) e capacidade antioxidante (DPPH). A melhor condição de extração acabou com a água: etanol (80:20), a 60 °C e por 30 min. A presença de ácidos fenólicos, flavonol glicosídeos e antocianinas (delfinidin-3-sambubiosídeo e cianidin-3-sambubiosídeo) foram identificados como sinais de maior intensidade. Com a secagem por pulverização a 150°Ce com G60/MD40, foi atingido o maior teor de fenóis e antocianinas totais, no entanto, a capacidade antioxidante foi favorecida a 150 °C e com G40/MD60. As microcápsulas obtidas podem ser utilizadas como matéria-prima na preparação de fitofarmacêuticos ou alimentos funcionais, considerando seu fácil manuseio, possível estabilidade e seu valor antioxidante.

Antioxidant Nano Phlorotannin Powder from Brown Algae Sargassum serratum: Spray Drying, Antioxidant Activities, Physic-Chemical Characterization

Introduction: Phlorotannins are bioactive-value polymers existing in brown algae and useful for pharmaceutics and functional food. Therefore, the study focused on the spray drying conditions survey, the evaluation of antioxidant activities, and physico-chemical characterization of antioxidant nano phlorotannin powder prepared from brown algae Sargassum serratum.Methods: To survey the effect of spray drying conditions (carriers, carrier-to-solution ratio, compressed air pressure, liquid feed speed, inlet air temperature) on antioxidant activities (total antioxidant, reducing power, DPPH free radical scavenging), and physico-chemical (solubility degree, moisture, particle morphology, and bulk density) of antioxidant phlorotannin powder from brown algae Sargassum serratumcommonly growing in the Vietnam sea area.Results: The optimum spray drying condition consisted of the carrier-to-solution ratio of 10%, compressed air pressure of 0.8 bar, the liquid feed speed of 10 ml min-1, and the inlet temperature of 110°C. At the optimization condition, the antioxidant activity of phlorotannin powder possessed total antioxidant (4.347 ± 0.018 g ascorbic acid equivalent 100-1g DP), reducing power activity (9.390 ± 0.024 g FeSO4equivalent 100-1g DP), DPPH free radical scavenging activity ((70.02 ± 0.26)%), physico-chemical of antioxidant phlorotannin powder consisting of moisture content (5 ± 0.5%), phlorotannin content (2.268 ± 0.010 g phloroglucinol equivalent 100-1g DP), solubility degree (100%), and bulk density (<1g/ml). Phlorotannin content and antioxidant activities were affected by the spray drying condition (p < 0.05) and a strong correlation to each other (R2> 0.9). Antioxidant phlorotannin particles possessed nanometer size and the morphology of irregular and microspheres.Conclusion: Antioxidant nano phlorotannin powder could be usefulas functional food and pharmaceuticals

Preparation of berberine hydrochloride dry powder inhalation and its effect on Staphylococcus aureus pneumonia / 中草药

Objective: To prepare berberine hydrochloride dry powder inhalation, and investigate its pharmacological effect on Staphylococcus aureus pneumonia after pulmonary administration. Methods: Berberine hydrochloride dry powder by spray drying and the experimental conditions was optimized by orthogonal experiment. The lung deposition, fluidity and appearance were characterized. The pharmacodynamic effects of the preparations on S. aureus pneumonia were performed with SD rats. Results: A berberine hydrochloride dry powder was prepared at an inlet temperature of 130 ℃ with a gas volume flow of 610 L/h and a feed volume flow of 3 mL/min. The berberine hydrochloride dry powder had a lung deposition rate (FPF) of 76.4% and an aerodynamic diameter of 4.61 μm. The stability index (SI) ≈ 1, the aeration energy ratio (AR) = 1.76 > 1, and the inflation energy (AE10) = 2.1 mJ < 10 mJ. Through the pharmacodynamic evaluation of S. aureus, we can know that the berberine hydrochloride dry powder inhalation effectively improved the pathological state of pneumonia rats, and significantly reduced (P < 0.05) the number of WBC, neutrophils, and the expression of inflammatory factors (TNF-α, IL-1β, and IL-6) in pneumonia rats. Conclusion: Berberine hydrochloride dry powder inhalation can directly reach the lesion site through pulmonary administration, so it has significant therapeutic effect on S. aureus pneumonia.

Extraction, characterization and microencapsulation of isoflavones from soybean molasses / Extração, caracterização e microencapsulação de isoflavonas do melaço de soja

ABSTRACT: This study aimed to extract isoflavones from soybean molasses with different solvents, furthermore, the selected extract, which showed overall desirable characteristics was selected to evaluate the potentials of different encapsulating agents. The encapsulating agents employed for the study included 18% Maltodextrin DE20 (T1), 18% Hi-maize (T2), and a mixture of equal proportions of 9% Maltodextrin DE20 and 9% of Hi-maize (T3). Solvents such as 80% ethanol and methanol, and grain alcohol in varying different concentrations of 50 and 80% were used for the studies. The best solvent for the extraction of phenolics and total isoflavones was 50% cereal alcohol, this extract also presented higher antioxidant activity. Evaluation of the encapsulating agents revealed that 18% Hi-maize with inlet air of 130 °C was best suited for the encapsulation of isoflavones. The ORAC method showed that microcapsules with the 18% Hi-maize encapsulating agent also had higher antioxidant activity.

RESUMO: Este estudo teve como objetivo extrair isoflavonas do melaço de soja com diferentes solventes, além disso, o extrato selecionado com as características desejáveis ​​em geral foi selecionado para avaliar os potenciais de diferentes agentes encapsulantes. Os agentes encapsulantes foram: 18% de maltodextrina DE20 (T1), 18% Hi-maize (T2) e uma mistura em proporções iguais de 9 % de maltodextrina DE20 e 9% de Hi-maize (T3). Foram testados os solventes, etanol e metanol a 80% e álcool de cereais a 50 e 80%. O melhor solvente para a extração de fenólicos e isoflavonas totais foi o álcool de cereais a 50%, sendo que este extrato também apresentou maior atividade antioxidante. Entre os agentes encapsulantes testados, 18% Hi-maize com ar de entrada de 130 °C mostrou ser o melhor para encapsular as isoflavonas. O método ORAC mostrou que as microcápsulas com o agente encapsulante Hi-maize a 18% também apresentaram maior atividade antioxidante.

Effect of Maltodextrin Concentration and Inlet Air Temperature on Properties of Spray Dried Powder from Reverse Osmosis Concentrated Sweet Orange Juice

Abstract Sweet orange juice is an important part of diet since it is nutritious beverage offering good taste and play significant part in a healthy diet. High hygroscopicity, thermo-plasticity and presence of low molecular weight components in sweet orange juice offer low glass transition temperature (Tg), likely to form soft particle with sticky surface leading to sticky powder during drying. Maltodextrins are amorphous drying aids that tend to inhibit sugar crystallization and form a high Tg product after drying. In this study, the effect of the different spray drying parameters on the quality of powder derived from control and concentrated juice at three inlet air temperatures 120, 130 and 140 °C and at three levels of juice total soluble solids (TSS): maltodextrin levels at 1:0.5; 1:1 and 1:1.5 were studied. The impact of inlet air temperature and maltodextrin concentration has significantly affected various properties of sweet orange powder. For control juice, process yields increased with increase in inlet air temperature and maltodextrin concentration. However, for reverse osmosis (RO) concentrate, process yield increased with increase in maltodextrin concentration and decreased with increase in inlet air temperature. For control juice, process yields obtained were in the range of 12.59-41.16% and in case of concentrated juice, the process yield obtained was in the range of 21.35-56.95% at different combinations of inlet air temperature and maltodextrin concentrations. Spray-dried powder was considered as "possible" and "fair" in terms of flowability and cohesiveness. Vitamin C retention was high at lower inlet air temperature with lower concentration of maltodextrin.

Bovine serum albumin-based nanoparticles containing the flavonoid rutin produced by nano spray drying

Rutin is a flavonoid compound obtained from different vegetables and fruits; specifically, it is found in the seeds of buckwheat and in fruit peels, particularly citrus. It is also an important constituent of red wine. Rutin exhibits various biological properties including antiviral, vasoprotective, anti-inflammatory, and anticarcinogenic activities. However, its antioxidant activity is the most well studied. Despite the potential for in vitro applications, rutin presents low oral bioavailability that affects its biological activities. Nanoparticles composed of polymers, protein, or lipids are of great importance in the pharmaceutical and nutraceutical areas due to their physicochemical properties, which improve the pharmacokinetics of the drug which is loaded within. This study presents the production of bovine serum albumin (BSA) nanoparticles containing rutin by nano spray drying. Nanoparticles were characterized in terms of mean particle size, size distribution, morphology, zeta potential, and drug content; as well as their antioxidant activity. The optimized spray-drying conditions produced spherical particles with a mean size of 316 nm, zeta potential of −32 mV, and encapsulation efficiency around 32%. Moreover, when antioxidant activity toward the ABTS+ radical was assayed, nanoencapsulation increased the IC50 of rutin by 2-fold. The nano spray-drying process proved to be suitable for the production of rutin-loaded BSA nanoparticles with potential antioxidant activity.

Formula Optimization of Rifampicin Dry Powder Inhalation with Chitosan-Xanthan Carrier Using Response Surface Methodology

This study was aimed to obtain an optimum formula of rifampicin dry powder inhalation (DPI) with chitosan-xanthan(CX) as a carrier by spray drying method using response surface methodology (RSM). Fourteen experimental formulaswere designed statistically by Box Behnken method by varying three parameters namely concentration of CX solution,rifampicin/CX ratio, and inlet temperature of the spray dryer. The entrapment efficiency (EE), particle size, and drugrelease in pH 7.4 (pulmonary condition) and pH 4.5 (pulmonary macrophages condition) of the rifampicin DPI werecharacterized. The optimum formula of rifampicin DPI was obtained using Design Expert software. The obtained DPIfrom those 14 formulas possessed EE of 112.00–149.08% and average particle sizes of 0.599–5.506 µm. Rifampicinrelease in phosphate buffer medium pH 7.4 was 6.54%–22.95% and in pH 4.5 was 12.02–48.60%. The DesignExpert predicted that the optimum formula would be obtained with a concentration of CX solution of 0.5%, a ratio ofrifampicin to CX 1:1, and inlet temperature of the spray dryer at 143°C. The optimized formula produced a rifampicinDPI with EE of 108.9%, the particle size of 1.177 µm, and the rifampicin release of 14.49% (at pH 7.4) and of 37.97%(at pH 4.5).

Spray drying technology of Shenpu Penyan Granule based on quality by design concept / 中草药

Design space approach was applied to optimize the spray drying process of Shenpu Penyan Granule (SPG) based on the concept of quality by design (QbD). The yield, moisture content, the content of paeoniflorin, chlorogenic acid, polydatin and salvianolic acid B were defined as the process critical quality attributes (CQAs). Based on the Plackett-Burman design, three critical process parameters (CPPs) including inlet temperature, specific gravity, and feeding speed were identified by using the weighted standardized partial regression coefficient method. And stepwise regression method was then used to establish the mathematical model between CQAs and CPPs in the Box-Behnken design. The variance analysis results showed that the P values of the five models were less than 0.05 and the mismatch values were all greater than 0.05, indicating that the model could describe the relationship between CQAs and CPPs. Probability based design space was obtained and verified using Monte-Carlo simulation method. According to the verification results, the robustness of first ethanol precipitation process of SPG can be guaranteed by operating within the design space parameters, which helps to improve the quality uniformity between batches of phenol extracts and provides data support for industrialization production.

Optimization of spray drying technology of Liqi Huoxue Compound extract by Box-Behnken response surface method combined with G1-entropy weight method / 中草药

Objective: To optimize the spray drying process of Liqi Huoxue Compound (LHC) extract and evaluate the quality of extract powder. Methods: The drug concentration, inlet air temperature and air flow were used as independent variables, and the comprehensive scores of ferulic acid, tanshinone IIA, salvianolic acid B, puerarin content and flour extraction rate were used as the response values, and the test data were binomial fitting. The mathematical relationship between the comprehensive scoring index and their respective variables was established, and Box-Behnken design-response surface method combined with G1-entropy weight method was used to optimize the spray drying process of LHC extract. Results: The optimal spray drying process was a specific solution gravity of 1.08, inlet air temperature of 140 ℃, and an air flow of 40 m3/h. Under such conditions, the average content of ferulic acid, tanshinone IIA, salvianolic acid B and puerarin by the spray drying was 0.300 4 mg/g, 0.338 0 mg/g, 18.526 0 mg/g and 7.508 8 mg/g, respectively. The flour yield was 81.49%, the overall score was 94.69, and the RSD value was 0.99%. Conclusion: The preferred spray drying process of LHC extract is stable and feasible.

Microencapsulated β-carotene preparation using different drying treatments / 浙江大学学报（英文版）（B辑：生物医学和生物技术）

β-Carotene is one of the most abundant natural pigments in foods; however, usage of β-carotene is limited because of its instability. Microencapsulation techniques are usually applied to protect microencapsulated β-carotene from oxidization. In this study, β-carotene was microencapsulated using different drying processes: spray-drying, spray freeze-drying, coating, and spray granulation. The properties of morphology, particle size, water content, thermal characteristic, and chemical stability have been explored and compared. Scanning electron microscopy measure¬ments showed that the coated powder had a dense surface surrounded by starch and suggested that the coating process gave a microencapsulated powder with the smallest bulk density and the best compressibility among the prepared powders. The chemical stabilities of microcapsules were evaluated during six months of storage at different temperatures. The coated powder had the highest mass fraction of β-carotene, which indicated that the coating pro¬cess was superior to the three other drying processes.

Preparation and Quality Evaluation of Zingiber officinale Oil Microcapsules / 中国药房

OBJECTIVE： To prepare Zingiber officinale oil microcapsules and to evaluate its quality. METHODS： Z. officinale oil microcapsules were prepared by spray drying method with sodium starch octenyl succinate as capsule material. The preparation technology was optimized by orthogonal test with mixing temperature of capsule material and capsule core， mass ratio of capsule material and capsule core， stirring speed as factors， using encapsulation efficiency as index. The drug loading， encapsulation efficiency， appearance， particle size distribution and stability of light， heat and humidity （using iodine value and peroxide value as indexes） were evaluated. RESULTS： The optimal preparation technology of Z. officinale oil microcapsules was that the mixing temperature of capsule material and core was 60 ℃； mass ratio of capsule material and capsule core was 10 ∶ 1； stirring speed was 12 000 r/min. Average drug-loading amount and encapsulation efficiency of Z. officinale oil microcapsules prepared by optimal technology were 17.97％ and 73.57％ （n＝3）. The morphology of Z. officinale oil microcapsules was round， smooth， non-sticky and uniform in size distribution. The average diameter of microcapsules was （6.30±0.27） μm. Under light， heat and humidity conditions， the iodine value and peroxide value of Z. officinale oil microcapsules changed slightly. CONCLUSIONS： The optimal preparation technology of Z. officinale oil microcapsules is simple and reproducible. The prepared microcapsules have good encapsulation efficiency， high drug loading amount and good stability.

Preparation Process and Formula of Kang'aiping Dispersible Tablets / 中国药学杂志

OBJECTIVE: To study preparation process and formula of Kang'aiping dispersible tablets. METHODS: Orthogonal designs were used to optimize water extraction process of traditional Chinese herbs from Kang'aiping pills, spray drying process of extracts and formulas of Kang'aiping dispersible tablets. RESULTS: The optimal water-extraction process is established by adding eight times water of raw materials, boiling for 60 min and extracting for two times. The optimal spray drying process parameters are that the density of the liquid extracts is 1.20 g•mL-1, inlet air temperature is 180 ℃ and outlet air temperature is 80 ℃. And the optimal formula consists of 37% microcrystalline cellulose, 5:1 of the ratio of croscarmellose sodium and PVPP, and 0.15% magnesium stearate. CONCLUSION: Formula and process optimized by using orthogonal experimental design is suitable for preparation of Kang'aiping dispersible tablets.

A new device for determination of adhesive force and its application in predicting hot-melt sticking in spray drying of traditional Chinese medicine / 中国中药杂志

A new device was designed to measure adhesive force and predict whether traditional Chinese medicine extracts would appear hot-melt sticking in spray drying process．Based on the physical property tester as fundamental test platform, the device was fixed with a camera, a temperature and humidity sensor probe and a set of equipment for hot air. This device could simulate the dry environment of spray dryer and analyze the variables of testing solutions' adhesiveness against drying time. To establish and validate a model of predicting hot-melt sticking in spray drying, data was collected by using data mining. The results of this study proved that the device could be used to predict the hot-melt sticking in spray drying based on the adhesive force of materials (testing solutions). In addition, the study also found that the adhesiveness of the hot-melt sticking materials gradually increased with the evaporation of water, while that of non-sticking materials first increased and then rapidly decreased.

Correlation between chemical compositions of traditional Chinese medicine extracts and phenomenon of wall stickiness in spray drying / 中国中药杂志

To explore the correlation between chemical compositions (organic acids, small molecule sugars, protein and others) of traditional Chinese medicine extracts and the wall stickiness in spray drying. In this study, 55 types of most common used Chinese herbs were selected to determine the content of 7 chemical components such as citric acid and fructose from plant extraction. The status of wall stickiness was observed during the drying process. The principle component analysis (PCA-X), hierarchical clustering analysis(HCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were then used to evaluate the correlation between each chemical compositions and wall stickiness, so as to look for the essential chemical compositions associated with the wall stickiness. All of the above 3 statistical analysis methods showed significant results in distinguishing the two groups (sticky or non-sticky). PCA-X score chart and HCA clustering scatter plot suggested that the small molecular substance was the main factor causing wall stickiness, which was then proved by the reality where some of the traditional herb extracts were in non-sticky state after drying but in sticky state after alcohol precipitation. OPLS-DA results revealed that L-malic acid, citric acid, fructose and glucose were the difference factors for the wall stickiness of the extracts. Under small molecular components, L-malic acid, citric acid, fructose and glucose were the crucial factors that directly led to the hot melt sticky wall of the herbal extracts, and macromolecular substances might ameliorate the function of wall stickiness.