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PubMed2001

Preparation and characterization of spray-dried oxidized cellulose microparticles.

The goal of this study was to investigate the feasibility of spray drying to produce microparticles of oxidized cellulose (OC), a biocompatible and bioresorbable polymer. OCs containing 7, 13, and 20 wt% carboxylic groups were converted into stable aqueous dispersions and then spray dried using a Yamoto G-32 spray dryer equipped with a standard fluid nozzle with an orifice of 406 microm. The following operating conditions were investigated: inlet temperature 140, 170, and 190 degrees C; feed rate 3, 6, and 9 mL/min; and atomization airpressure 0.5, 1, and 1.5 kg f/cm2. The amounts of OC used in feed were 1, 2.5, and 5%. OC microparticles produced under these conditions were shrunken spheres, ranging in size between 0.98+/-0.47 and 2.05+/-0.98 microm. The different operating conditions used had no significant effect on the size and shape of particles. The use of a water-soluble plasticizer (glycerin, polyethylene glycol 400, or polyethylene glycol 6000) in the dispersion yielded microparticles with a good sphericity and a smooth surface morphology, whereas no change in the shape or size of microparticles was noted with water-insoluble plasticizers, Triacetin and dibutyl phthalate. Powder X-ray diffraction and Fourier transform infrared spectral analyses of spray-dried microparticles showed no change in the solid-state structure of OC. In conclusion, results show that OC can be converted into stable aqueous dispersions and used to produce microparticles by spray drying.

Capsules↗
PubMed2006

The apparent plasticizing effect of polyethylene glycol (PEG) on the crystallinity of spray dried lactose/PEG composites.

Aqueous solutions of lactose and polyethylene glycol (PEG) were spray dried in a Büchi Model 191 spray dryer with the aim to investigate the effect of PEG on the crystallinity of the composite. A PEG concentration of 10.7% by weight of solids was studied for PEG 200, 600, 1500, 4000 and 8000. For PEG 200 and 4000 additional concentrations from 1.5-19.3% to 1.5-32.4%, respectively, were investigated. The spray dried composites were analysed with X-ray powder diffraction and modulating differential scanning calorimetry. The crystallinity of lactose in the composites varied from 0% to 60%, dependent on the molecular weight and concentration of PEG. Apparently, lactose crystallinity is promoted by low molecular weight and high concentration of the PEG. PEG did not affect the lactose glass transition temperature. It is suggested that lactose and PEG are solidified separately during spray drying and that partial crystallization of lactose is associated with effects of PEG on the rate of drying.

Calorimetry, Differential Scanning↗
PubMedDate not supplied

Application of a spray drying technique in the production of TRH-containing injectable sustained-release microparticles of biodegradable polymers.

Copoly (dl-lactic/glycolic acid) microparticles for sustained release of a water-soluble drug (Thyrotropin releasing hormone: TRH) were prepared by a spray drying method. A higher entrapment ratio was achieved with the spray drying method with the in-water drying method. In order to avoid agglomeration of the microparticles, a double-nozzle spray drying method was designed using mannitol as an anti-adherent. The surface of the spray-dried microparticles was coated with mannitol, and the extent of agglomeration was decreased. Acetonitrile was the most suitable solvent for microencapsulation using the double-nozzle spray drying method because the initial burst of TRH from the microparticles during the first day was the smallest. When PLGA with a weight-average molecular weight of 14,000 was used, constant release of TRH continued for one month with a small initial burst. In conclusion, the production of biodegradable microparticles by the double-nozzle spray drying method appears to be an attractive alternative to conventional microencapsulation methods.

Biodegradation, Environmental↗
PubMed2003

Field activity and storage stability of Anagrapha falcifera nucleopolyhedrovirus (AfMNPV) in spray-dried lignin-based formulations.

A multiple-embedded nucleopolyhedrovirus isolated from Anagrapha falcifera (Kirby) (AfMNPV) has potential to be developed into a microbial bioinsecticide because the host range includes several economic pests. We tested spray-dried AfMNPV formulations after storage for insecticidal activity based on bioassays with neonate Trichoplusia ni (Hübner). Eight experimental lignin-based spray-dried formulations, a glycerin-based formulation, and an unformulated sample were made with virus stock from three commercial production lots. Samples of these formulations were stored at 30 degrees C in individually sealed sample containers for destructive sampling after 1, 3, and 6 mo whereas the remaining product was stored in glass jars under refrigeration for up to 30 mo. Spray drying did not significantly reduce the initial LC50s of AfMNPV in experimental formulations compared with unformulated virus that was not spray dried. Refrigerated storage for 6 mo did not significantly lower virus activity of formulated samples compared with the unformulated AfMNPV stored frozen, while samples stored for 30 mo had higher LC50 values determined by both droplet and leaf feeding assays. When stored at 30 degrees C, most formulations (22 of 24) maintained insecticidal activity for 3 mo, but most (21 of 24) lost significant activity after 6 mo of storage. The glycerin-based formulation also lost activity within 6 mo of storage at 30 degrees C when compared with frozen unformulated virus, but did not lose activity when stored refrigerated for up to 30 mo. These formulations were evaluated after 7 mo at 4 degrees C for residual insecticidal activity when applied to field grown cabbage. Insecticidal activity was determined against T. ni neonates for treated leaf samples collected at 3, 7, 27, and 51 h after application of 2.5 x 10(12) obs/ha. Field tests showed no differences in activity among samples of stored formulations and one freshly made formulation. Spray-dried formulations had significantly higher insecticidal activity (67.5% mortality) compared with the unformulated treatment (30% mortality) sampled 3 h after application. At 3, 7, and 27 h after application, the spray-dried formulations had higher residual activity (67%, 59%, and 42% mortality, respectively), compared with the commercial glycerin-based formulation (61%, 38%, and 23% mortality, respectively). These experiments demonstrated that AfMNPV in lignin-based spray-dried formulations had a shelf-life of up to 3 mo at 30 degrees C and up to 30 mo at 4 degrees C, and with longer residual insecticidal activity in the field compared with unformulated or a glycerin formulation.

Animals↗
PubMed2003

Etanidazole-loaded microspheres fabricated by spray-drying different poly(lactide/glycolide) polymers: effects on microsphere properties.

In this work, a spraying technique was used to encapsulate etanidazole (a hypoxic radiosensitizer) into different poly(lactide/glycolide) polymers. The properties of the obtained microspheres, especially the particle size and distribution, morphology and release rate were investigated. Unexpectedly, poly(L-lactide) (PLLA) shows a fast release rate, comparable to PLGA 50: 50, due to the dissociation of the microspheres although the release rate of the spray-dried microspheres of other polymers decreases with increasing lactide ratio. It is also interesting to note that, contrary to the viscosity sequence of the polymer solutions, the particle size of the microspheres decreases in the order PLGA 50: 50, PLGA 65: 35, PLGA 85: 15 and PDLA. The morphology of microspheres can be affected by polymer properties (e.g. lactide/glycolide ratio, molecular weight, crystallinity and Tg) and fabrication conditions (e.g. solvent and polymer concentration to be sprayed). Although most of the microspheres fabricated by EA have a donghnut-like shape with smooth surface, it is possible to obtain spherical particles by choosing proper polymer type and polymer concentration. A further examination of the mechanisms of the atomization process and the solvent evaporation process reveals their respective effect on droplet formation and particle formation, both of which are essential for the spray-drying technique. It is found that polymer phase transition (affected by the polymer solubility) and its subsequent solvent evaporation processes can finally determine the morphology and the particle size of the spray-dried particles made from different polymers. In essence, the lactide/glycolide ratio of the polymers plays a more important role in affecting the properties of the spray-dried microspheres.

Biocompatible Materials↗
PubMed2004

Process characteristics and compaction of spray-dried emulsions containing a drug dissolved in lipid.

The objective of the present study is to prepare directly compressible powders, containing a poorly water-soluble drug dissolved in medium-chain triglycerides (MCT), by spray drying o/w-emulsions in a pilot plant spray dryer. In addition to the lipid phase, the emulsions contained a water-soluble carrier (a sugar), a water-insoluble carrier (magnesium alumino metasilicate) and a combined emulsifier and film-forming agent (gelatine). A factorial design was used to investigate the effect of formulation variables on the spray drying process and powder properties. The factors varied were soluble carrier type (trehalose or mannitol), insoluble carrier particle size distribution (granular or fine powder) and amount of lipid phase in the emulsion (low or high). Compressibility and compactibility of the spray-dried emulsions were mainly affected by the content of lipid in the powders and decreased on increasing the amount of lipid. Increasing the particle size of the insoluble carrier decreased spray drying process yield and lipid encapsulation efficiency whereas compactibility and handling properties were improved. Incorporation of a soluble carrier becoming amorphous on spray drying resulted in tablets with an increased mechanical strength compared to powders containing a crystalline soluble carrier.

Emulsions↗
PubMed1999

Spray-dried bovine blood: an effective laboratory diet for Ctenocephalides felis felis (Siphonaptera: Pulicidae).

Commercially available spray-dried protein sources were evaluated as replacement laboratory cat flea, Ctenocephalides felis felis (Bouché), larval diets for slaughterhouse-collected heat-dried blood. Percentage of adult emergence of fleas reared on adult flea feces (87.7%) and spray-dried bovine blood (79%) did not significantly differ, and yeast supplementation did not significantly increase adult emergence for spray-dried diets. However, yeast supplementation of heat-dried blood increased percentage adult emergence from 0 to 41.7%. Spray-dried bovine blood was found to be a satisfactory laboratory diet for cat flea larvae.

Animals↗
PubMed2004

Theophylline particle design using chitosan by the spray drying.

Solid dispersions of theophylline with chitosan as a carrier were prepared using a spray-drying method. Chitosan dissolved in an acid solution forms a gel, but it does not dissolve in an alkaline solution. Therefore, drugs which form composite particles with chitosan would gradually be released in an acid solution, and are expected to have considerably sustained release in an alkaline solution. In this study, we aimed to apply this ability to sustained release pharmaceutics. In this study, we used theophylline as a model drug and chitosan as a carrier. Mixtures of chitosan and the drug in prescribed ratios were dissolved in an acid solution. The physicochemical properties of the solid dispersions obtained were investigated by powder X-ray diffraction, differential scanning calorimetry, and dissolution rate analyses, with a view to clarify the effect of crystallinity on the dissolution rate. Furthermore, the interaction between the drug and the carrier was investigated by FT-IR analysis. The powder X-ray diffraction intensity of the drug in the spray-dried samples decreased with an increase in chitosan contents, which also caused changes from crystalline to amorphous forms. These results indicated that the system formed a solid dispersion. The dissolution profiles of the drug from the physical mixtures and solid dispersions were almost the same at pH 1.2. However, at pH 6.8, the release from the solid dispersions was sustained more than that from the physical mixtures. The FT-IR spectroscopy for the theophylline solid dispersions suggested that the carbonyl group of theophylline and the amino group of chitosan formed a hydrogen bond. Mass median aerodynamic diameter (MMAD) was measured by using a cascade impactor to evaluate the possibility of solid dispersions as dry powder inhalations. The MMAD of the spray-dried theophylline-chitosan systems were 4.5-5.0 microm. The results suggested that the spray-drying method is usefull to produce dry powders for inhalation.

Calorimetry, Differential Scanning↗
PubMed2003

Investigation of the physical properties of spray-dried stabilised lysozyme particles.

The aim of this study was to investigate the effect of the composition of formulations on the physical properties, including glass-transition temperatures (Tg) and aerodynamic-related characteristics, of spray-dried lysozyme particles. The Tg, as determined by differential scanning calorimetry, of spray-dried lysozyme formulations was found to be dependent upon the type and amount of excipient(s) included in the formulation. In addition, the Tg of sucrose-containing particles appeared to be raised markedly by the inclusion of trehalose, but not by dextran. The surfaces of all spray-dried particles were shown by scanning electron microscopy to be smooth with some containing characteristic dimples, typical of spray-dried material, and the morphology appeared to be independent of variation in excipient composition. However, the volume median diameters (VMD) of spray-dried powders, as determined by laser diffraction, were found to depend upon the amounts of excipients. The fine particle fraction of enzyme delivered to the lower stage of a twin-stage impinger from lysozyme-trehalose 1:1 powders appeared to be greater than that from lysozyme-sucrose 1:1 particles (22.5% vs 15.9%) when dispersed via a Rotahaler although a similar dispersibility of the two formulations (39.6% vs 36.7%) was found from a glass inhaler. In general, spray-drying was demonstrated to be feasible to produce respirable particles of the stabilised model protein, with Tg of the formulations being > 30 degrees C higher than room temperature.

Crystallization↗
PubMed1999

Stability and surface activity of lactate dehydrogenase in spray-dried trehalose.

The stability of the model protein lactate dehydrogenase (LDH) during spray-drying and also on subsequent dry storage was examined. Trehalose was used as a carrier. The spray-drying temperatures Tinlet and Toutlet have a measurable effect on LDH inactivation. Low Tinlet produced the least process inactivation, but gave a high residual moisture content making the protein's storage stability poor. High Tinlet reduced residual moisture and improved storage stability, but at the cost of high process inactivation. As already found for other systems, addition of a surfactant (in this case polysorbate 80) could ameliorate process inactivation of LDH at Tinlet = 150 degreesC. Surfactant had, however, a deleterious effect on storage stability of LDH, the vital factor being the molar ratio of surfactant/protein in the dried product. By using electron spectroscopy it was shown that LDH has a 10 times higher surface concentration in the dried trehalose particles than expected for a homogeneous distribution. Surface tension measurements at the water/air interface proved that LDH is surface active, although the Gibbs equation appeared to be inapplicable. Calculations of spray-droplet formation time and drying time indicate than the extent of diffusion-driven LDH adsorption to the liquid/air interface is sufficient to account for the measured amount of LDH inactivation during spray-drying. The presence of 0.1% polysorbate 80 to the spray solution prevents LDH from appearing at the surface of the dried particles. As a negative control, the phosphatide Lipoid E 80 does not prevent the appearance of LDH in the surface according to electron spectroscopy and does not therefore prevent LDH inactivation during spray-drying at Tinlet = 150 degreesC.

Animals↗
PubMed1988

Preparation of biodegradable poly(+/-)lactide microparticles using a spray-drying technique.

Drug containing biodegradable poly(+/-)lactide microparticles were prepared by using a spray-drying technique. Formulations containing model drugs in either a dissolved (progesterone) or dispersed state (theophylline) were spray-dried. The spray-drying method was less dependent on the solubility characteristics of the drug when compared with traditional microencapsulation techniques such as phase separation or solvent evaporation techniques. Differential scanning calorimetry and scanning electron microscopy were used to characterize the microparticles. The drug release profiles were characterized by a rapid release phase (burst effect) followed by a slow release phase, the extent of each phase being dependent on the drug loading.

Biodegradation, Environmental↗
PubMed2002

Bacteriocin production by spray-dried lactic acid bacteria.

AIMS: Cell survival and antagonistic activity against Listeria innocua, Listeria monocytogenes and Staphylococcus aureus were investigated after spray-drying three bacteriocin-producing strains of lactic acid bacteria: Carnobacterium divergens, Lactobacillus salivarius and Lactobacillus sakei. METHODS AND RESULTS: Bacterial cell concentrates were spray-dried and stored at 4 degrees C and 18 degrees C and 0.3% ERH (equilibrium relative humidity). Enumeration and antagonistic activity were evaluated before and after spray-drying and at regular intervals during storage. CONCLUSIONS: A higher survival rate was obtained when survival was performed at 4 degrees C. With the exception of Carnobacterium divergens which lost the inhibitory activity against Staph. aureus after drying, antagonistic production was not affected by the process nor by the storage. Of the three species studied, Lact. salivarius showed the highest resistance to the spray-drying and storage processes. SIGNIFICANCE AND IMPACT OF THE STUDY: Spray-drying is a potentially useful process for large scale production of dried powders containing viable organisms with antagonistic activity against pathogens.

Aerosols↗
PubMed2005

Preparation and evaluation of glibenclamide-polyglycolized glycerides solid dispersions with silicon dioxide by spray drying technique.

Solid dispersions (SDs) of glibenclamide (GBM); a poorly water-soluble drug and polyglycolized glycerides (Gelucire with the aid of silicon dioxide (Aerosil 200); as an adsorbent, were prepared by spray drying technique. SDs and spray dried GBM in comparison with pure GBM and corresponding physical mixtures (PMs) were initially characterized and then subjected to ageing study up to 3 months. Initial characterization of SDs and spray dried GBM by DSC and XRPD showed that GBM was present in its amorphous form (AGBM). Improvement in the solubility and dissolution rate was observed for all samples. DRIFT spectroscopy revealed presence of hydrogen bonding in SDs. During ageing study, almost no decrease of in vitro drug dissolution was observed, over the period of 3 months as compare with freshly prepared SDs. Slight crystallinity in SDs was observed in the DSC and XRPD studies during ageing. Moreover in vivo study in Swiss Albino mice also justified the improvement in the therapeutic efficacy of amorphous GBM in SDs over pure GBM. Thus, present study demonstrated the high potential of spray drying technique for obtaining stable free flowing SDs of poorly water-soluble drugs using polyglycolized glycerides carriers with the aid of silicon dioxide as an adsorbent.

Animals↗
PubMed1995

Added dietary methionine in starter pig diets containing spray-dried blood products.

Two experiments were conducted to determine the dietary methionine requirement of weanling pigs fed diets containing spray-dried porcine plasma and(or) blood meal in a phase-feeding program. In Exp. 1, 216 crossbred pigs (21 +/- 2 d of age and 4.9 kg BW) were fed diets (1.6% lysine, .52% cystine) containing 10% spray-dried porcine plasma and 1.75% spray-dried blood meal from d 0 to 21 postweaning. Pigs were fed one of six dietary treatments ranging from .28 to .48% total dietary methionine (.225 to .425% apparent digestible methionine). From d 0 to 14 and d 0 to 21 postweaning, ADG, ADFI, and gain:feed ratio (G:F) increased (quadratic, P < .01) as dietary methionine increased. Inflection point analysis projected .42 and .41% total dietary methionine to maximize ADG and G:F from d 0 to 14 and d 0 to 21 postweaning, respectively. In Exp. 2,216 crossbred pigs (21 +/- 3 d of age and 5.6 kg BW) were used to determine the dietary methionine requirement from d 7 to 28 postweaning. All pigs were fed the same diet (1.6% lysine, .44% methionine, .52% cystine) from d 0 to 7 postweaning. From d 7 to 28, pigs were assigned to one of six dietary treatments (1.3% lysine, .46% cystine) containing 10% dried whey and 3% spray-dried blood meal. Total dietary methionine levels ranged from .27 to .42% (.249 to .399% apparent digestible methionine). From d 7 to 14 postweaning, increasing dietary methionine increased (quadratic, P < .05) ADG, ADFI, and G:F (.34 to .35% total methionine projected by inflection point analysis).(ABSTRACT TRUNCATED AT 250 WORDS)

Amino Acids, Essential↗
PubMed2002

Comparison of spray-dried blood meal and blood cells in diets for nursery pigs.

We used a total of 680 pigs to compare spray-dried blood meal and blood cells in nursery diets. In Exp. 1, 350 barrows (17 +/- 2 d of age at weaning) were used to compare three levels of spray-dried blood meal or blood cells (2.5, 5.0, and 7.5%) in the diet fed from d 5 to 19 postweaning (6.6 to 9.9 kg). Inclusion of either blood product improved ADG (P < 0.005) and G:F (P < 0.001) compared to pigs fed the control diet without added blood products. However, pigs fed spray-dried blood meal had greater ADG (P < 0.001), ADFI (P < 0.04), and G:F (P < 0.001) from d 0 to 7 compared to those fed blood cells. The greatest differences observed between the two blood products occurred at the 5 and 7.5% inclusion levels. No differences (P > 0.05) in growth performance were detected between the two blood products from d 7 to 14. In Exp. 2, 380 barrows (initial BW of 10.7 kg and 41 +/- 2 d of age) were used to determine lysine bioavailability of spray-dried blood meal and blood cells via the slope ratio procedure. With G:F ratio as the response criterion, blood meal and blood cells had similar lysine bioavailability relative to crystalline lysine. These experiments indicate that both blood products had similar lysine bioavailability, and that pigs fed spray-dried blood meal had greater performance during the initial 7 d (d 5 to 12 after weaning). However, as the pigs became heavier, there were no differences observed in performance of pigs fed either blood meal or blood cells.

Animal Feed↗
PubMed2005

The influence of formulation components on the aerosolisation properties of spray-dried powders.

Dry powders suitable for inhalation containing beta-estradiol, leucine as a dispersibility enhancer and lactose as a bulking agent were prepared by spray-drying from aqueous ethanol formulations. The influence of formulation components on the characteristics of the resultant spray-dried powders was examined through the use of a range of ethanol concentrations (10-50% v/v) in the solvent used to prepare the initial formulations. Additionally, the amount of leucine required to act as a dispersibility enhancer was investigated by varying the amount of leucine added to the formulation prior to spray-drying. Following spray-drying, resultant powders were characterised using scanning electron microscopy, laser diffraction and tapped density measurements, and the aerosolisation performance determined using Twin Stage Impinger and Andersen Cascade Impactor analysis. We demonstrate that selection of appropriate solvent systems and leucine concentration allows the preparation of spray-dried powders that display enhanced aerosolisation properties, and would be predicted to exhibit high deposition in the lower regions of the respiratory tract.

Administration, Inhalation↗
PubMed2003

Secondary structure of cyclosporine in a spray-dried liquid crystal by FTIR.

The conformational state of cyclosporine in liquid crystalline spray-dried powders and the solution structure of cyclosporine, in a series of organic solvents where solvent dipole and hydrogen bonding ability varied, were determined. Fourier transformed infrared spectra (FTIR) were obtained on cyclosporine powders, and cyclosporine solutions in a series of organic solvents. Tetragonal crystalline cyclosporine revealed an intermolecular aggregate band at 1614 cm(-1), a beta-sheet band at 1627 cm(-1), a gamma-loop band at 1648 cm(-1), a gamma-turn band at 1658 cm(-1) (formed from a hydrogen bond between D-Ala(8)NH and MeLeu(6)Cdbond;O) and a Type II beta-turn band at 1673 cm(-1) (centered at the hydrogen bond betweenVal(5)NH to Abu(2)Cdbond;O). A similar conformation was observed in chloroform or octanol (apolar), where a second beta-sheet band emerged at 1638 cm(-1) and a turn structure associated with the beta-OH on MeBmt(1) appeared at 1685 cm(-1). However, the spray dried liquid crystal structure resembled the solution conformation in acetone or acetonitrile (hydrogen bond acceptor). The conformation in acetone suggested that the beta-sheet, gamma-loop, Type II beta-turn and MeBmt(1) turn remained intact. Interestingly, the spray-dried powder conformations did not resemble the solution structure of the solvent (ethanol) from which they had been obtained. The conformation in ethanol and methanol (hydrogen bond donor) showed only beta-sheet, gamma-turn, MeBmt(1) turn structure. Only a small population of molecules retained the Type II beta-turn. Finally, cyclosporine is essentially insoluble in water, so the water conformation has never been elucidated; however, a conformation resembling the active structure was obtained in a cosolvent solution containing both hydrogen bond donors and acceptors. This conformation is in good agreement with molecular modelling studies where cyclosporine is docked in the active site of cyclophilin. Spray-dried cyclosporine formed a liquid crystal that can be described as maintaining the Type II beta-turn, beta-sheet, and gamma-loop structures seen in crystalline material. However, the hydrogen bond between D-Ala(8)NH and MeLeu(6)Cdbond;O was disrupted.

Cyclosporine↗