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Residual Solvents (residual + solvent)
Selected AbstractsCarbon dioxide extraction of residual chloroform from biodegradable polymersJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 5 2002Wendy S. Koegler Abstract Biodegradable polymeric devices for drug delivery and tissue engineering are often fabricated with the use of organic solvents and may still contain significant amounts of solvent (> 1 wt%) even after aggressive vacuum drying. This excess solvent can interfere with tissue response and the mechanical properties of the devices. The aim of this article is to demonstrate that liquid CO2 extraction can be used to reduce residual solvent in dense poly(L -lactide-co-glycolide) devices to 50 ppm relatively quickly and with minimal changes in architecture under some conditions. Two liquid CO2 extraction systems were developed to examine the removal of residual solvents from bar-shaped PLGA devices: (1) a low-pressure (1400 psi) batch system, and (2) a high-pressure (5000 psi) continuous-flow system. Eight hours of extraction in the high-pressure system reduced residual chloroform in 3 mm thick bars below the 50-ppm target. A simple Fickian diffusion model was fit to the extraction results. Diffusion coefficients ranged from 1.10×10,6 cm2/s to 2.64×10,6 cm2/s. The model predicts that ,1 h is needed to dry 1-mm bars to chloroform levels below 50 ppm, and 7 h are needed for 3 mm thick bars. The micro- and macroarchitectures of porous PLGA scaffolds created by particulate leaching were not significantly altered by CO2 drying if the salt used to make the pores was not removed before drying. © 2002 Wiley Periodicals, Inc. J Biomed Mater Res (Appl Biomater) 63: 567,576, 2002 [source] EFFECT OF DIRECT APPLICATIONS OF SAGE (SALVIA OFFICINALIS L.) LEAVES ON OXIDATIVE STABILITY OF SUNFLOWER OIL DURING ACCELERATED STORAGEJOURNAL OF FOOD QUALITY, Issue 5 2009EDA ÇALIKO ABSTRACT In this study, various sage applications were examined on oxidative stability of sunflower oil during accelerated storage. There are three applications: (1) direct sage leaves (S); (2) deodorized sage leaves (DeS); and (3) essential oil of sage leaves. The main compounds of essential oil were identified as, -thujone (35.87%),, -thujone (14.41%), 1,8-cineol (10.59%) and camphor (10.09%). Oxidative stability of these three applications was tested by Schall Oven test at 60C applying peroxide value and conjugated dienes, and Rancimat at 110C. Whereas the highest antioxidants activity was found for 2% S followed by 0.5% S and 2% DeS, all sage treatments statistically retarded the oxidation compared with the control sample. The most appealing result was that the residue can be used as a natural antioxidants. That means the reuse of residue may decrease economic losses and health risk in comparison with synthetic antioxidants and extracts because it is completely natural and contains no residual solvent. PRACTICAL APPLICATIONS While almost all of previous studies were concentrated on the use of herb extracts, our study investigates the results of direct application of sage on oxidation. Especially with this study, we have evaluated a possible application area for sage residue leftover after the deodorization process. [source] Ketoprofen nanoparticle gels formed by evaporative precipitation into aqueous solutionAICHE JOURNAL, Issue 7 2006Xiaoxia Chen Abstract Aqueous nanoparticle gels of a poorly-water soluble drug, ketoprofen, were produced by evaporative precipitation into aqueous solution (EPAS). Liquid droplets of surfactant stabilized ketoprofen containing residual solvent were dispersed in water from 60 to 90°C below the melting point of pure ketoprofen. The carboxylic acid group in ketoprofen dissociates in pure water, providing electrostatic stabilization of the droplets to complement steric stabilization. Stable amorphous ketoprofen particles with a mean size of 135 nm, measured by dynamic light scattering, were formed with only 0.1% w/v poloxamer 407, resulting in an exceptionally high drug-to-surfactant ratio of 10:1. For 5% w/v poloxamer 407, interactions with ketoprofen produced a bluish, transparent gel composed of ,50 nm particles. In 2 min, 98% of the ketoprofen in the gel nanoparticles dissolved. The favorable interactions between the ketoprofen and poloxamer 407, along with the electrostatic and steric stabilization, lead to gelation, which further stabilizes the unusually small particles. The rapidly dissolving wet gels with extremely small particle sizes, one month stability, and relatively low viscosities, are of interest in transdermal and parenteral delivery; furthermore, the gels may be dried for oral delivery. © 2006 American Institute of Chemical Engineers AIChE J, 2006 [source] Freeze-drying of tert- butanol/water cosolvent systems: A case report on formation of a friable freeze-dried powder of tobramycin sulfateJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 4 2002Sakchai Wittaya-Areekul Abstract A case study is presented in which a tert -butanol (TBA)/water cosolvent system was found to be a useful means of producing freeze-dried tobramycin sulfate that readily forms a loose powder upon agitation in a specialized application in which a critical quality attribute is the ability to pour the sterile powder from the vial. Both formulation and processing variables are important in achieving acceptable physical properties of the cake as well as minimizing residual TBA levels. Liquid/liquid phase separation was observed above critical concentrations of both drug and TBA, resulting in a two-layered lyophilized cake with unacceptable appearance, physical properties, and residual TBA levels. However, the choice of tobramycin sulfate and TBA concentrations in the single-phase region of the phase diagram resulted in a lyophilized solid that can readily be poured from vials. Crystallization of TBA before drying is critical to achieving adequately low residual TBA levels, and this is reflected in the effect of thermal history of freezing on residual TBA levels, where rapid freezing results in incomplete crystallization of TBA and relatively high levels of residual solvent. Annealing at a temperature above T,g of the system after an initial freezing step significantly reduces the level of residual TBA. Secondary drying, even at increased temperature and for extended times, is not an effective method of reducing residual TBA levels. © 2002 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 91: 1147,1155, 2002 [source] Development of electronic nose method for evaluation of residual solvents in low-density polyethylene films ,PACKAGING TECHNOLOGY AND SCIENCE, Issue 2 2007Isinay E. Yüzay Abstract Flexible packaging films containing high levels of residual volatile organic compounds (VOCs) can alter the flavour and odour of packaged foods. Currently, a range of gas chromatographic techniques and sensory evaluations are used for assessing the residual VOCs in packaging films. An objective method for assessing the residual solvents from low-density polyethylene (LDPE) was developed using an Alpha MOS Fox 3000 electronic nose (e-nose) equipped with 12 metal oxide semiconductor sensors. Three VOCs, ethyl acetate, ethyl alcohol and toluene, were chosen as models for solvents of interest in flexible food packaging analysis. LDPE film samples were spiked with single and binary mixtures of solvents and analysed using the e-nose and by GC,FID (HP 6890; Hewlett-Packard Co., Wilmington, DE). The responses obtained from the e-nose were processed using principal component analysis (PCA) and discriminate factorial analysis (DFA) in order to identify the residual solvents. Partial least squares analysis (PLS) was also used to quantify the amount of residual solvent and to correlate the e-nose results with gas chromatography, which is currently the standard method for determining residual VOCs in packaging films. There was good agreement between the e-nose responses and gas chromatography results for single solvents (r = 0.90,0.98). The technique also worked for binary solvent mixtures (r = 0.84,0.99). The electronic nose can be a viable alternative to traditional techniques while providing simplicity and objectivity, which would be extremely advantageous in routine quality control of residual solvents. Copyright © 2006 John Wiley & Sons, Ltd. [source] Principles of risk assessment for determining the safety of chemicals: Recent assessment of residual solvents in drugs and di(2-ethylhexyl) phthalateCONGENITAL ANOMALIES, Issue 2 2004Ryuichi Hasegawa ABSTRACT Risk assessment of chemicals is essential for the estimation of chemical safety, and animal toxicity data are typically used in the evaluation process, which consists of hazard identification, dose,response assessment, exposure assessment, and risk characterization. Hazard identification entails the collection of all available toxicity data and assessment of toxicity endpoints based on findings for repeated dose toxicity, carcinogenicity or genotoxicity and species-specificity. Once a review is compiled, the allowable lifetime exposure level of a chemical is estimated from a dose,response assessment based on several measures. For non-carcinogens and non-genotoxic carcinogens, the no-observed-adverse-effect-level (NOAEL) is divided by uncertainty factors (e.g. with environmental pollutants) or safety factors (e.g. with food additives) to derive a tolerable daily intake (TDI) or acceptable daily intake (ADI), respectively. These factors include interspecies and individual differences, duration of exposure, quality of data, and nature of toxicity such as carcinogenicity or neurotoxicity. For genotoxic carcinogens, low dose extrapolation is accomplished with mathematical modeling (e.g. linearized multistage model) from the point of departure to obtain exposure levels that will be associated with an excess lifetime cancer risk of a certain level. Data for levels of chemicals in food, water and air, are routinely used for exposure assessment. Finally, risk characterization is performed to ensure that the established ,safe' level of exposure exceeds the estimated level of actual exposure. These principles have led to the evaluation of several existing chemicals. To establish a guideline for residual solvents in medicine, the permitted daily exposure (PDE), equivalent to TDI, of N,N-dimethylformamide was derived on the basis of developmental toxicity (malformation) and of N-methylpyrrolidone on the basis of the developmental neurotoxicity. A TDI for di(2-ethylhexyl)phthalate was derived from assessment of testicular toxicity. [source] Carbon dioxide extraction of residual chloroform from biodegradable polymersJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 5 2002Wendy S. Koegler Abstract Biodegradable polymeric devices for drug delivery and tissue engineering are often fabricated with the use of organic solvents and may still contain significant amounts of solvent (> 1 wt%) even after aggressive vacuum drying. This excess solvent can interfere with tissue response and the mechanical properties of the devices. The aim of this article is to demonstrate that liquid CO2 extraction can be used to reduce residual solvent in dense poly(L -lactide-co-glycolide) devices to 50 ppm relatively quickly and with minimal changes in architecture under some conditions. Two liquid CO2 extraction systems were developed to examine the removal of residual solvents from bar-shaped PLGA devices: (1) a low-pressure (1400 psi) batch system, and (2) a high-pressure (5000 psi) continuous-flow system. Eight hours of extraction in the high-pressure system reduced residual chloroform in 3 mm thick bars below the 50-ppm target. A simple Fickian diffusion model was fit to the extraction results. Diffusion coefficients ranged from 1.10×10,6 cm2/s to 2.64×10,6 cm2/s. The model predicts that ,1 h is needed to dry 1-mm bars to chloroform levels below 50 ppm, and 7 h are needed for 3 mm thick bars. The micro- and macroarchitectures of porous PLGA scaffolds created by particulate leaching were not significantly altered by CO2 drying if the salt used to make the pores was not removed before drying. © 2002 Wiley Periodicals, Inc. J Biomed Mater Res (Appl Biomater) 63: 567,576, 2002 [source] 1H and 13C NMR data to aid the identification and quantification of residual solvents by NMR spectroscopyMAGNETIC RESONANCE IN CHEMISTRY, Issue 6 2005Ian C. Jones Abstract We present reference data and a javascript web page which allow the rapid identification and quantification of residual solvents by NMR. The data encompass all of the ICH-prescribed solvents and were obtained for a number of NMR solvents. We also present an example of its application. Copyright © 2005 John Wiley & Sons, Ltd. [source] Development of electronic nose method for evaluation of residual solvents in low-density polyethylene films ,PACKAGING TECHNOLOGY AND SCIENCE, Issue 2 2007Isinay E. Yüzay Abstract Flexible packaging films containing high levels of residual volatile organic compounds (VOCs) can alter the flavour and odour of packaged foods. Currently, a range of gas chromatographic techniques and sensory evaluations are used for assessing the residual VOCs in packaging films. An objective method for assessing the residual solvents from low-density polyethylene (LDPE) was developed using an Alpha MOS Fox 3000 electronic nose (e-nose) equipped with 12 metal oxide semiconductor sensors. Three VOCs, ethyl acetate, ethyl alcohol and toluene, were chosen as models for solvents of interest in flexible food packaging analysis. LDPE film samples were spiked with single and binary mixtures of solvents and analysed using the e-nose and by GC,FID (HP 6890; Hewlett-Packard Co., Wilmington, DE). The responses obtained from the e-nose were processed using principal component analysis (PCA) and discriminate factorial analysis (DFA) in order to identify the residual solvents. Partial least squares analysis (PLS) was also used to quantify the amount of residual solvent and to correlate the e-nose results with gas chromatography, which is currently the standard method for determining residual VOCs in packaging films. There was good agreement between the e-nose responses and gas chromatography results for single solvents (r = 0.90,0.98). The technique also worked for binary solvent mixtures (r = 0.84,0.99). The electronic nose can be a viable alternative to traditional techniques while providing simplicity and objectivity, which would be extremely advantageous in routine quality control of residual solvents. Copyright © 2006 John Wiley & Sons, Ltd. [source] Reactivity of ethyl acetate and its derivatives toward ammonolysis: ramifications for ammonolysis-based microencapsulation processPOLYMERS FOR ADVANCED TECHNOLOGIES, Issue 10 2009Younglim Chung Abstract The reactivity of three ester organic solvents toward ammonolysis was examined in relation to the development of an ammonolysis-based microencapsulation process. Ethyl acetate, ethyl chloroacetate, and ethyl fluoroacetate were chosen as ester organic solvents. Progesterone was considered as a model drug to be encapsulated into poly- D, L -lactide- co -glycolide microspheres. A polymeric dispersed phase was emulsified in an aqueous phase, to which ammonia was added to initiate ammonolysis. The polarization status of a carbonyl group in the backbone of the ester was found to decide the magnitude of the ester reactivity. In fact, the simple ester ethyl acetate hardly reacted with ammonia, while ethyl chloroacetate and ethyl fluoroacetate showed greater reactivity toward ammonolysis. The rapid completion of ammonolysis led to the conversion of the water-immiscible solvents into water-soluble solvents, thereby providing an efficient tool for microsphere solidification. Among microencapsulation parameters, the type of dispersed solvent, the molar ratio of ammonia to a dispersed solvent, and the percentage of the progesterone payload decisively influenced the characteristics of the microspheres. Subsequently, variations in such parameters accompanied considerable influence on microsphere morphology, incorporation efficiency, thermal behavior, the degree of residual solvents, and the physical status of progesterone. Optimization of the process parameters would not only contribute to improving the ammonolysis-based microencapsulation process, but would also permit the tailoring of microsphere properties to specific demands. Copyright © 2008 John Wiley & Sons, Ltd. [source] | |||||||||||||