Optimization of Process Parameters using Response Surface Methodology for the Removal of Zinc(II) by Solvent Extraction

A factorial design of experiments and a response surface methodology were implemented to investigate the liquid-liquid extraction process of zinc (II) from acetate medium using the 1-Butyl-imidazolium di(2-ethylhexyl) phosphate [BIm+][D2EHP-]. The optimization process of extraction parameters such as the initial pH effect (2.5, 4.5, and 6.6), ionic liquid concentration (1, 5.5, and 10 mM) and salt effect (0.01, 5, and 10 mM) was carried out using a three-level full factorial design (33). The results of the factorial design demonstrate that all these factors are statistically significant, including the square effects of pH and ionic liquid concentration. The results showed that the order of significance: IL concentration > salt effect > initial pH. Analysis of variance (ANOVA) showing high coefficient of determination (R2 = 0.91) and low probability values (P < 0.05) signifies the validity of the predicted second-order quadratic model for Zn (II) extraction. The optimum conditions for the extraction of zinc (II) at the constant temperature (20 °C), initial Zn (II) concentration (1mM) and A/O ratio of unity were: initial pH (4.8), extractant concentration (9.9 mM), and NaCl concentration (8.2 mM). At the optimized condition, the metal ion could be quantitatively extracted.

New Simultaneous High Performance Liquid Chromatographic Method for Determination of NSAIDs and Opioid Analgesics in Advanced Drug Delivery Systems and Human Plasma

A new and cost effective RP-HPLC method was developed and validated for simultaneous analysis of non steroidal anti inflammatory dugs Diclofenac sodium (DFS), Flurbiprofen (FLP) and an opioid analgesic Tramadol (TMD) in advanced drug delivery systems (Liposome and Microcapsules), marketed brands and human plasma. Isocratic system was employed for the flow of mobile phase consisting of 10 mM sodium dihydrogen phosphate buffer and acetonitrile in molar ratio of 67: 33 with adjusted pH of 3.2. The stationary phase was hypersil ODS column (C18, 250×4.6 mm i.d., 5 μm) with controlled temperature of 30 C°. DFS in liposomes, microcapsules and marketed drug products was determined in range of 99.76-99.84%. FLP and TMD in microcapsules and brands formulation were 99.78 - 99.94 % and 99.80 - 99.82 %, respectively. Single step liquid-liquid extraction procedure using combination of acetonitrile and trichloroacetic acid (TCA) as protein precipitating agent was employed. The detection limits (at S/N ratio 3) of quality control solutions and plasma samples were 10, 20, and 20 ng/ml for DFS, FLP and TMD, respectively. The Assay was acceptable in linear dynamic range. All other validation parameters were found in limits of FDA and ICH method validation guidelines. The proposed method is sensitive, accurate and precise and could be applicable for routine analysis in pharmaceutical industry as well as in human plasma samples for bioequivalence and pharmacokinetics studies.

Contamination of Organochlorine Pesticides in Nest Soil, Egg, and Blood of the Snail-eating Turtle (Malayemys macrocephala) from the Chao Phraya River Basin, Thailand

Organochlorine pesticides (OCPs) are known to be persistent and bioaccumulative toxicants that may cause reproductive impairments in wildlife as well as human. The current study uses the snail-eating turtle Malayemys macrocephala, a long-lived animal commonly distribute in rice field habitat in central part of Thailand, as a sentinel to monitor OCP contamination in environment. The nest soil, complete clutch of eggs, and blood of the turtle were collected from agricultural areas in the Chao Phraya River Basin, Thailand during the nesting season of 2007-2008. The novel methods for tissue extraction by an accelerated solvent extractor (ASE, for egg) and liquid-liquid extraction (for blood) have been developed. The nineteen OCP residues were analyzed by gas chromatography with micro-electron captured detector (GC-μECD). The validated methods have met requirements of the AOAC standard. The results indicated that significant amounts of OCPs are still contaminated in nest soil and eggs of the turtle even though the OCPs had been banned in this area for many years. This suggested the potential risk to health of wildlife as well as human in the area.

Influence of Electrolytes and High Viscosity on Liquid-Liquid Separation

Liquid-liquid extraction is a process using two immiscible liquids to extract compounds from one phase without high temperature requirement. Mostly, the technical implementation of this process is carried out in mixer-settlers or extraction columns. In real chemical processes, chemicals may have high viscosity and contain impurities. These impurities may change the settling behavior of the process without measurably changing the physical properties of the phases. In the current study, the settling behavior and the affected parameters in a high-viscosity system were observed. Batchsettling experiments were performed to experimentally quantify the settling behavior and the mixer-settler model of Henschke [1] was used to evaluate the behavior of the toluene + water system. The viscosity of the system was increased by adding polyethylene glycol 4000 to the aqueous phase. NaCl and Na2SO4 were used to study the influence of electrolytes. The results from this study show that increasing the viscosity of water has a higher influence on the settling behavior in comparison to the effects of the electrolytes. It can be seen from the experiments that at high salt concentrations, there was no effect on the settling behavior.

n-Butanol as an Extractant for Lactic Acid Recovery

Extraction of lactic acid from aqueous solution using n-butanol as an extractant was studied. Effect of mixing time, pH of the aqueous solution, initial lactic acid concentration, and volume ratio between the organic and the aqueous phase were investigated. Distribution coefficient and degree of lactic acid extraction was found to increase when the pH of aqueous solution was decreased. The pH Effect was substantially pronounced at pH of the aqueous solution less than 1. Initial lactic acid concentration and organic-toaqueous volume ratio appeared to have positive effect on the distribution coefficient and the degree of extraction. Due to the nature of n-butanol that is partially miscible in water, incorporation of aqueous solution into organic phase was observed in the extraction with large organic-to-aqueous volume ratio.

A New Correlation for Overall Sherwood Number in Packed Liquid-Liquid Extraction Column

Using plug flow model in conjunction with experimental solute concentration profiles, overall volumetric mass transfer coefficient based on continuous phase (Koca), in a packed liquid-liquid extraction column has been optimized. Number of 12 experiments has been done using standard system of water/acid acetic/toluene in a 6 cm diameter, 120 cm height column. Thorough consideration of influencing parameters we intended to correlate dimensionless parameters in term of overall Sherwood number which has an acceptable average error of about 15.8%.