Cloud Point Extraction Technique Research Articles

Sustainable Recovery of Polyphenols and Carotenoids from Horned Melon Peel via Cloud Point Extraction.

Using natural plant extracts as food additives is a promising approach for improving food products' quality, nutritional value, and safety, offering advantages for both consumers and the environment. Therefore, the main goal of this study was to develop a sustainable method for extracting polyphenols and carotenoids from horned melon peel using the cloud point extraction (CPE) technique, intending to utilize it as a natural food additive. CPE is novel promising extraction method for separation and pre-concentration of different compounds while being simple, inexpensive, and low-toxic. Three parameters within the CPE approach, i.e., pH, equilibrium temperature, and equilibrium time, were investigated as independent variables through the implementation of Box-Behnken design and statistical analyses. The optimized conditions for the maximum recovery of both polyphenols and carotenoids, reaching 236.14 mg GAE/100 g and 13.80 mg β carotene/100 g, respectively, were a pH value of 7.32, an equilibrium temperature of 55 °C, and an equilibrium time of 43.03 min. The obtained bioactives' recovery values under the optimized conditions corresponded to the predicted ones, indicating the suitability of the employed RSM model. These results highlight the effectiveness of CPE in extracting bioactive compounds with varying polarities from agricultural by-products, underscoring its potential for enhancing the value of food waste and advancing sustainable practices in food processing. According to microbiological food safety parameters, the optimal CPE extract is suitable for food applications, while its storage under refrigerated and dark conditions is particularly beneficial. The CPE extract's enhanced stability under these conditions makes it a more viable option for long-term storage, preserving both safety and quality.

Plackett–Burman screening of physico-chemical variables affecting Citrus peel-mediated synthesis of silver nanoparticles and their antimicrobial activity

With the growing resistance of pathogenic microbes to traditional drugs, biogenic silver nanoparticles (SNPs) have recently drawn attention as potent antimicrobial agents. In the present study, SNPs synthesized with the aid of orange (Citrus sinensis) peel were engineered by screening variables affecting their properties via Plackett–Burman design. Among the variables screened (temperature, pH, shaking speed, incubation time, peel extract concentration, AgNO3 concentration and extract/AgNO3 volume ratio), pH was the only variable with significant effect on SNPs synthesis. Therefore, SNPs properties could be enhanced to possess highly regular shape with zeta size of 11.44 nm and zeta potential of − 23.7 mV. SNPs purified, capped and stabilized by cloud point extraction technique were then checked for their antimicrobial activity against Bacillus cereus, Listeria innocua, Listeria monocytogenes, Staphylococcus aureus, Enterobacter cloacae, Escherichia coli, Klebsiella pneumoniae, Pseudomonas aeruginosa, Salmonella typhimurium and Candida albicans. The maximum antimicrobial activity of SNPs was recorded against E. coli, L. monocytogenes and C. albicans with clear zone diameter of 33.2, 31.8 and 31.7 mm, respectively. Based on minimum inhibition concentration and minimum bactericidal concentration of SNPs (300 mg/l) as well as their effect on respiratory chain dehydrogenases, cellular sugar leakage, protein leakage and lipid peroxidation of microbial cells, E. coli was the most affected. Scanning electron microscopy, protein banding and DNA fragmentation proved obvious ultrastructural and molecular alterations of E. coli treated with SNPs. Thus, biogenic SNPs with enhanced properties can be synthesized with the aid of Citrus peel; and such engineered nanoparticles can be used as potent antimicrobial drug against E. coli.

Exploring the Antioxidant Properties of Citrus limon (Lemon) Peel Ultrasound Extract after the Cloud Point Extraction Method

Each year, a substantial amount of food is discarded around the globe. A significant portion of this waste consists of by-products derived from Citrus fruits such as lemons. The purpose of this research is to examine the polyphenol extraction and the antioxidant ability of lemon peel using cloud point extraction (CPE), a sustainable approach. CPE was conducted using three steps with a 20% w/v concentration of Span 20 as the surfactant, which has a critical micellar concentration of 6.13 × 10−5 mol/L. The pH was set at 7 and a salt concentration of 20% was maintained at 45 °C for 20 min. The subsequent outcomes of the analysis were obtained: total polyphenol content (TPC): 526.32 mg gallic acid equivalents per liter; total flavonoid content (TFC): 90.22 mg rutin equivalents per liter; FRAP, DPPH, and hydrogen peroxide assays: 2.40, 2.68 and 1.03 mmol ascorbic acid equivalents per liter, respectively, and 168.63 mg/L ascorbic acid content. The quantification of the polyphenolic compounds through High-Performance Liquid Chromatography showed that the most abundant compounds in the lemon peels are eriocitrin (159.43 mg/L) and hesperidin (135.21 mg/L). The results indicate that the proposed CPE technique is successful in extracting antioxidant compounds from lemon peels. The generated extracts have the potential to be exploited as dietary additives to enhance human health and can also be utilized for nutraceuticals or pharmaceutical purposes.

Two Spectrophotometric Methods Based on Diazotization Coupling Reaction for Determination of Genistein in Pure and Supplement

Genistein (GEN) is one of the predominant dietary isoflavones found in legumes such as soybeans. Genistein has been recommended as an osteoporosis treatment for postmenopausal women and elderly men, with the intention of reducing cardiovascular disease and hormone-dependent malignancies. Therefore, two sensitive and simple methods for quantifying it in the supplements preparation were developed.The first method (A) comprised employing the surfactant Triton X-114 to extract the result of the diazotization reaction with 4-Aminoacetophenone(4AMA) utilizing a cloud point extraction technique. The product was extracted using micelles of a non-ionic surfactant (TritonX-114) and then spectrophotometrically detected at a specified wavelength of 437nm. The linearity of the calibration curve was in the range of 0.25 -2.75 µg/mL of GEN(r = 0.9978) under optimal conditions. The average sample recovery was determined to be between 96 and 101 %. For 2 µg/mL of GEN, the relative standard deviation (RSD) was (0.27%). The second method (B) involved using the spectrophotometric-flow injection methodology for the same diazotization coupling reaction described above, and the orange colored dyewas measured at a wave length of 437 nm.Calibration curve were linear at different concentration range of GEN 10 to 100 µg/mL , relative standard deviation RSD% were 0.23 to 1.21. The proposed methods were applied to determine the presence of GEN in Supplements.

Separation and Micro Determination of Zinc(II) and Cadmium(II) in Food Samples Using Cloud Point Extraction method

The cloud point extraction technique has become increasingly popular in recent years for trace metal separation and preconcentration. When heated to a specific temperature, cloud point extraction utilizes the property of nonionic surfactants in aqueous solutions to generate micelles and become turbid (so-called cloud point temperature). For analytical chemists, developing a simple and selective technology for the separation and determination of metals and medicinal drugs is a critical concern. Therefore, a sensitive, accurate, and green cloud point extraction (CPE) procedure was developed for the micro-determination of metal cations like zinc (II) and cadmium (II) in food samples. Triton X–114 and 1-(4-(Phenyldiazenyl) phenyl) azo naphthalene-2-ol (Sudan III) were used as extractants. Sudan III forms an ion-pair association complex with metal ions when the pH is 9. In the presence of 5 ppm zinc (II) or 4 ppm cadmium (II) in an aqueous solution, the maximum extraction efficiency should be achieved. In order to create Cloud Point Temperature (CPT) quantitatively, the extraction applications in this approach required heating at 85°C for 20 minutes. In this work, the impacts of different surfactants, pH, stoichiometry, and various organic reagents on interferences as well as spectrophotometric determination were explored. The linearity ranges of zinc (II) and cadmium (II) were 0.25-700 and 0.25-400 ppm, respectively. The results show low detection limits of 0.035 and 0.042 ppm for zinc (II) and cadmium (II), respectively. Also, the quantification limits for zinc (II) and cadmium (II) are 0.116 and 0.140 ppm, respectively.

Development of a Cloud Point Extraction Technique Based on Lecithin for the Recovery of Carotenoids from Liquid Tomato Wastewater

The traditional extraction methods used to recover natural antioxidants from food industry wastes involve significant amounts of hazardous solvents. A viable alternative is the use of non-toxic surfactants to remove organic compounds from wastes at temperatures above the cloud point. Cloud point extraction has only recently begun to be used to recover high-value added compounds from food industry wastes. In the current work, a method for the isolation of high-value added components from liquid tomato wastewater using a cloud point extraction method was developed and optimized. Food-grade lecithin was examined for its potential to be used as a surfactant in the developed procedure. Moreover, parameters affecting the extraction (ionic strength, sample pH, temperature of extraction, and surfactant concentration) were examined and optimized. According to the results, the maximum recovery of carotenoids from the sample could be achieved with the developed procedure, by simply adjusting the pH to 3.5, adding 35.6% (w/v) sodium chloride, and setting the temperature at 45 °C. Moreover, the amount of lecithin used was examined. In order to extract the total amount of carotenoids from a sample, it was found that either three extractions with 1% lecithin are needed, or two extractions with 2% lecithin. In addition, the antioxidant activity of the extract was examined and it was found to scavenge 36.3% of DPPH free radicals. This percentage was 10% lower compared to the initial sample, which suggests that the extracted compounds retain their activity. Overall, the developed procedure can be used to recover carotenoids in a cost-efficient and easy way.

Displacement cloud point extraction procedure for preconcentration of iron(III) in water and fruit samples prior to spectrophotometric determination

ABSTRACT. For the enrichment of iron(III) prior to spectrophotometric determination, displacement cloud point extraction (D-CPE) technique was applied depending on the difference in stability constant of metal complexes. Zinc(II) as gallic acid complex was first separated into a Triton X-100 surfactant. Then, once the aqueous phase has been removed, the sample containing Fe(III) is added, and another CPE process is performed. Because Fe-GA has a higher stability than Zn-GA, Fe(III) can displace Zn(II) from the pre-extracted Zn-GA, allowing for Fe(III) separation from the complex sample matrix and its spontaneous spectrophotometric determination at 560 nm. The effects of pH, ligand, and surfactant quantities, temperature and heating time, centrifuge processes, and interferences were all studied. At the optimal conditions, the calibration graph was linear from 0.5 to 500 µg L-1 with enrichment factor of 75.0. The LOD was 0.15 µg L-1 and the RSD was 1.3% for 60 µg L-1 of Fe(III), n = 10. Accuracy was also evaluated using the standard reference substance (SRS) and flame atomic absorption spectroscopy (FAAS) approaches. This procedure was used for separation and micro-determination of Fe(III) in water and fruit tests (banana, strawberry, lemon, orange, and peaches) with recoveries ranged from 96.5 to 105%.
 
 KEY WORDS: Displacement cloud point extraction, Iron, Spectrophotometry, Fruit samples
 
 Bull. Chem. Soc. Ethiop. 2023, 37(1), 1-10. 
 DOI: https://dx.doi.org/10.4314/bcse.v37i1.1 

Spectrophotometric Analysis of Vancomycin Hydrochloride in Pure and Pharmaceutical Injections via Batch and Cloud Point Extraction Techniques

Development of a precise and delicate reaction has been acquired for the determination of vancomycin hydrochloride using batch and cloud point extraction (CPE) methods. The first method is based on the formation of azo dye as a result of diazotized dapsone coupled with vancomycin HCl (VAN) in a basic medium. The sensitivity of this reaction was enhanced by utilizing a nonionic surfactant (Triton X-114) and the cloud point extraction technique (second method). The azo dye formed was extracted into the surfactant-rich phase, dissolved in ethanol and detected at λmax 440 nm spectrophotometrically. The reaction was investigated using both batch and CPE methods (with and without extraction), and a simple comparison between the two developed methods was made. The conditions that affect the extraction process and the sensitivity of the methods have been carefully examined. The linearity of the calibration curves was in the range of 3-50 and 0.5- 25 µg.mL-1 with limits of detection of 0.806 and 0.462 µg.mL-1 for VAN in both batch and CPE procedures, respectively. The percentage of relative standard deviation (R.S.D.%) for the two methods was better than 2.54% and 2.83%, respectively. The recommended procedures have been effectively used to assay VAN in commercial injections.

ADSORPTIVE MICELLAR FLOCCULATION AND CLOUD POINT EXTRACTION AS PRE-CONCENTRATION METHODS FOR THE DETERMINATION OF PHENOSAFRANINE DYE IN AQUEOUS SOLUTIONS

A micellar-based preconcentration method for the extraction of Phenosafranine (PS) dye was developed by using adsorptive micellar flocculation (AMF) and cloud point extraction (CPE) techniques. In the case of AMF, aluminum sulphate (flocculant) and sodium dodecyl sulphate (SDS) were taken in 1:2 ratios for the extraction of PS dye. The parameters affecting the AMF and CPE were optimized. The calibration range and detection limits were 0.0-8.07 g/mL and 4.182 g/mL respectively for AMF. The calibration range and detection limits were 0.0-9.684 g/mL and 2.272ng/mL respectively for CPE.s The methods presented were used to extract PS dye from aqueous samples.

New microextraction methods for the evaluation of bromhexine HCl in pure and pharmacological formulations.

In this study, ion-pair reactions were used to investigate bromhexine HCl. The development of simple, accurate, sensitive, low-cost, and efficient extraction methods for bromohexine HCl separation, such as the DLLME and cloud point extraction techniques, are described as bromhexine HCl estimation methodologies. These methods employed the interaction of bromohexine HCl with alizarin yellow reagent to produce a yellow complex in an acidic medium (pH = 5). The complex's maximum absorbance intensity was 480 nm, and the stoichiometry for both continuous variation and molar ratio methods was determined to be 1:1. The dispersive liquid liquid microextraction (DLLME) method's concentration range (1-23µg.mL-1), the Beers law was obeyed with correlation coefficient (R2=0.998), limit of detection as (0.055µg.mL-1), limit of quantification as (0.183µg.mL-1) and molar absorptivity as (23930.2L.mol-1.cm-1).In the second technique, the cloud pointextraction method, The linearity of calibration curve above was the range between (1-40 µg.mL-1), the correlation coefficient (R2=0.998) and molar absorptivity was (13202.88L.mol-1.cm-1), (LOD) and (LOQ) were (0.141µg.mL-1) and (1.4641µg.mL-1), respectively. The proposed techniques can be used for the determination of bromohexine HCl in both pure and pharmaceutical formulations with very good success and pharmaceutical formulations with very good success.

Spectroscopic Estimation of Cefepime by using Batch, Cloud Point extraction and Flow Injection Analysis methods

The purpose of the study new simple, quick and sensitive spectrophotometric methods for determination of cefepime (CFM) in pure and Pharmaceutical Formulations. The primary amine was converted to an azo-dye coupling in the alkaline medium by 2,6 -dimethylphenol for stable reddish-orange color at a wave length of 515 nm. The concentration ranges 2-50 μg / mL, Beer's law is obeyed, the correlation coefficient, molar absorptivity , detection limit were 0.9996,0.826×104and 0.192 respectively .To estimation the trace concentration of dye used cloud point extraction (CPE) technique , followed by UV-Vis spectrophotometer .Detailed analysis and a series of ideal conditions were carried out on the influence of several parameters, such as surfactant form and volume, salt, temperature and incubation times on the cefepime CPE. The concentration range obeyed the Beer's law was 0.25-10 μg / mL, correlation coefficient was 0.9997, molar absorptivity was 1.169×105 L.mol-1.cm-1, detection limit was 0.027 μg/mL, Pre-concentration factor was 25 and Distribution coefficient(D) was 332.35. A flow injection analysis it’s simple technique for determination the cefepime. The concentration ranges 1-150 μg / mL, Beer's law is obeyed, correlation coefficient was 0.9997, molar absorptivity was 0.341×104L.mol-1.cm-1 and the detection limit was 0.464 μg/mL. For the determination of cefepime in pharmaceutical formulation the methods suggested were successfully used.

Determination of Trace Nitrite Amounts in Soil by Developed Cloud Point Extraction-Spectrophotometry Method

A new and simple method for the selective and sensitive determination of trace amounts of nitrite in soil samples is developed by a combination of cloud point extraction (CPE) and spectrophotometry technique. The procedure is based on the Griess reaction on 3,3`-dimethyl benzidine with nitrite in the presence of 1-naphthol in acidic media to form a yellow diazo dye, which shows absorption at lambda max 455 nm. The formation of colored diazo dye is followed by extraction into the Triton X-114-rich phase. CPE method parameters such as surfactant amount, temperature, and incubation time are evaluated and optimized. The results showed a very good linear range of 10-1250 µgL-1, with good regression coefficients (R2) ≥ 0.9997 and a preconcentration factor of 12.5. The limit of detection (LOD) describes as 3SDblank/m, and the limit of quantification (LOQ) describes as 10SDblank/m, where ‘m’ is the slope of the calibration curve and they are equal to 7.50 and 22.71 µgL-1 respectively. The recommended method can apply to determine the ultra-trace amount of nitrite in soil samples.

Evaluation of salbutamol in pure form and pharmaceutical formulations using spectrophotometry and green nonionic surfactant of cloud point extraction

The purpose of the study was to identify a quick, simple and sensitive spectrophotometric technique for the assessment of salbutamol (SAL). The proposed approach depends on SAL’s azo-coupling reaction with BEN. The orange color of the reaction product was analyzed at λmax (480 nm) against a blank solution. It was obeyed to beer-lambert show over concentration between (2.5-17.5 mg.L−1) with LOD (1.283 mg.L−1), LOQ (4.234 mg.L−1) and molar absorptivity (12922.74 L.mol−1.cm−1). The procedure revealed high sensitivity for assessment of chosen drug. The new cloud point extraction technique was also successfully utilized for the extraction of pharmaceutically pure SAL drug, (also known as 2-[4-(2,4,4-trimethylpentan-2-yl) phenoxy] ethanol), was selected as green extraction solvent due to its properties and structure. The influence of various parameters, such as the kind and volume of surfactant, salt, temperature and incubation time on the CPE of salbutamol was investigated in detail and a set of perfect conditions was established. A correlation coefficient (R2) was 0.9914 for the calibration curve was obtained. The LOD, LOQ and molar absorptivity were 0.041 mg.L−1, 0.12 mg.L−1 and 47024.61 L.mol−1.cm−1, respectively. We believe that our suggested method is rapid, very convenient, and cost effective for the determination of salbutamol drug in the various samples.

Optimization of the extraction of antioxidants from winery wastes using cloud point extraction and a surfactant of natural origin (lecithin)

Cloud Point Extraction (CPE) technique was used to recover phenolic compounds from wine sludge wastes using lecithin as a surfactant. Lecithin is a safe natural product with no toxicity and, therefore, no separation of recovered phenolic substances from the surfactant system is required to use them in food systems. A progressive optimization sequence involving multiple recovery stages (up to three), various surfactant concentrations (2, 5, 10, 15% w/v), different temperatures (35–55 °C) and pH values (2.5–5.0) was followed to optimize the CPE procedure. The efficiency of the CPE procedure after altering the above parameters was determined by the recovery of polyphenols after CPE procedure. According to the results, a surfactant concentration of 5%, the use of multiple CPE steps, a pH value of 3 and a temperature of 40 °C were the optimal conditions for the separation of phenolic compounds from wine sludge using lecithin as a surfactant. In addition, the antioxidant activity of the extracts was determined using various methods, namely DPPH•, Rancimat and Differential Scanning Calorimetry. The surfactant rich phases (which include the polyphenols extracted from the waste) showed high antioxidant activity.

Studying the effect of an ionic liquid on cloud point extraction technique for highly efficient preconcentration and speciation analysis of tellurium in water, soil and sediment samples

A simple, novel and highly sensitive ionic liquid-assisted cloud point extraction (IL-CPE) and preconcentration method was developed for the determination and speciation analysis of tellurium, using 1-octyl-3-methylimidazolium chloride as an additive for improving the extraction efficiency of Triton X-114. The Te(IV) species was complexed with ammonium pyrrolidine dithiocarbamate, extracted into the micellar IL/surfactant phase and then directly measured by electrothermal atomic absorption spectrometry (ETAAS). The total Te concentration was obtained after a pre-reduction step and Te(VI) concentration was calculated as the difference between total Te and Te(IV). Several parameters, including the type and concentration of IL and surfactant, time and temperature of the IL-CPE procedure and ETAAS conditions were thoroughly evaluated and optimized. In addition, the action mechanism of the IL on CPE was studied by fluorescence measurements using Laurdan as a polarity probe. The decrease in the internal polarity caused by the incorporation of the IL into the micelles was responsible for the improvement in the extraction efficiency. Under the optimized conditions, a sensitivity enhancement factor of 87 and an extraction efficiency of 90% were achieved. Limits of detection of 1.1 and 1.7 ng L−1 and relative standard deviations of 3.9% and 5.0% for Te(IV) and Te(VI), respectively, were obtained. The developed IL-CPE method was successfully applied for Te speciation analysis in matrices of different complexities, such as waters (tap, underground and seawater), soil and sediment.

Determination of Lisinopril in Bulk and Pharmaceutical Formulations by Cloud Point Extraction—A Green Method

A sensitive and eco-friendly method was developed for the spectrophotometric determination of Lisinopril (LSP) in bulk and pharmaceutical formulations by cloud point extraction technique. The method was based on the formation of a blue-colored coordination complex between Lisinopril (LSP) and Cobalt Thiocyanate (CTC) at a suitable pH. The Complex in aqueous medium was extracted into surfactant layer by cloud point extraction using a non-ionic surfactant Triton X-114 and then the surfactant layer was dissolved in a suitable volume of ethanol and the amount of Lisinopril was determined spectrophotometrically at a wavelength of 625 nm. The conditions like concentration of the drug, concentration of CTC and of Triton X-114, PH, etc. were optimized by OFAT (One Factor At a Time) method. The linear range of calibration curve was 1 - 6 μg/ml and the linear regression equation with a correlation coefficient of 0.99996 was y = 0.0021 + 0.084x. Preconcentration and enrichment factors were found to be 100 and 3.12 respectively, achieving the detection limit of 0.0588 μg/ml. The proposed method was successfully applied for the determination of LSP in the drug formulations. The obtained values were in agreement with the values as quoted by the manufacturers.

Purification and Fractionation of Carbon Dots using pH-controlled Cloud Point Extraction Technique

In this work, we describe a simple, green and general procedure for the purification and fractionation of carbon dots (CDs). CDs coated with oxygen-containing functional groups were synthesized by thermal pyrolysis of citric acid. The product of the reaction was first Purified and then fractionated into two distinct kinds of CDs (f4 and f1) using pH-controlled cloud point extraction (CPE) technique. Characterization of f4 and f1 fractions by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-Vis absorption, and FT-IR spectroscopy not only lead to study and explain the mechanism of the extraction procedure but also revealed that the two fractions were different from each other in terms of their different optical properties and surface chemistry (the number or surface-density of oxygen-containing functional groups) which in turn plays the main role in their fractionation at different pH values. Comparing fluorescence spectra of f4 and f1 fractions indicated that the surface-density or number of the oxygen-containing functional groups has a marked effect on photoluminescence behavior of CDs. The developed general procedure method can be used for large-scale production of different fractions of any pure CDs in the industry as well as research laboratory preparation purposes.

Micro Spectrophotometric Determination and Cloud Point Extraction of Sulphadimidine Sodium in Pure form and Pharmaceutical Drug

Two simple, rapid, and useful spectrophotometric methods were suggest or the determination of sulphadimidine sodium (SDMS) with and without using cloud point extraction technique in pure form and pharmaceutical preparation. The first method was based on diazotization of the Sulphdimidine Sodium drug by sodium nitrite at 5 ºC, followed by coupling with α –Naphthol in basic medium to form an orange colored product . The product was stabilized and its absorption was measured at 473 nm. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.03012 μg∙cm-1, the detection limit was 0.0277 μg∙ml-1, and the limit of Quantitation was 0.03605μg∙ml-1.The second method was the cloud point extraction (CPE) using Trtion X-114 as surfactant. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.02958 μg∙cm-1, the detection limit was 0.01745 μg∙ml-1, and the limit of quantitation was 0.028303 μg∙ml-1. All variables including the reagent concentration, reaction time, color stability period, and mole ratio were studied in order to optimize the reaction conditions. The mole ratio for the composition of product is (1:1). Both methods were effectively useful to the determination of sulphdimidine sodium in pharmaceutical dose form. The attained results were in a good agreement with the official and other methods in the literature .No interference were observed from the commonly encountered additives and excipients.

Micro Spectrophotometric Determination and Cloud Point Extraction of Sulphadimidine Sodium in Pure form and Pharmaceutical Drug

Two simple, rapid, and useful spectrophotometric methods were suggest or the determination of sulphadimidine sodium (SDMS) with and without using cloud point extraction technique in pure form and pharmaceutical preparation. The first method was based on diazotization of the Sulphdimidine Sodium drug by sodium nitrite at 5 ºC, followed by coupling with α –Naphthol in basic medium to form an orange colored product . The product was stabilized and its absorption was measured at 473 nm. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.03012 μg∙cm-1, the detection limit was 0.0277 μg∙ml-1, and the limit of Quantitation was 0.03605μg∙ml-1.The second method was the cloud point extraction (CPE) using Trtion X-114 as surfactant. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.02958 μg∙cm-1, the detection limit was 0.01745 μg∙ml-1, and the limit of quantitation was 0.028303 μg∙ml-1. All variables including the reagent concentration, reaction time, color stability period, and mole ratio were studied in order to optimize the reaction conditions. The mole ratio for the composition of product is (1:1). Both methods were effectively useful to the determination of sulphdimidine sodium in pharmaceutical dose form. The attained results were in a good agreement with the official and other methods in the literature .No interference were observed from the commonly encountered additives and excipients.

A new approach for separation and recovery of betaine from beet molasses based on cloud point extraction technique.

The aim of this work was to explore the possibility of the application of cloud point extraction (CPE) method in micelle media to recovery betaine from beet molasses. Response surface method was employed to assess the effects of surfactant concentration, molasses concentration, incubation time, pH, electrolyte concentration, mixing time, and surfactant type on efficiency of betaine recovery from beet molasses. Also, a mathematical model was developed to predict the effect of each variable and their interactions on the efficiency of betaine recovery. The model showed that best surfactant was Triton X-114 and under the optimum conditions, betaine recovery from beet molasses was achieved up to 80% when three CPE steps with total of 1.5% (w/v) of surfactant were used. Subsequently, betaine was recovered nearly 100% from surfactant rich phase after adjusting pH at 2.5 and re-incubation at 40°C. The results showed that the proposed method is suitable for extraction of betaine from beet molasses.