scholarly journals Preconcentration and determination of Metformine Hydrochloride in different samples by cloud point extraction coupling with uv-visible spectrophotometry

2016 ◽  
Vol 13 (2) ◽  
pp. 470-479
Author(s):  
Baghdad Science Journal

This work was influenced the separation and preconcentration steps were carried out to determination of metformin (MET) in pharmaceutical preparations and human serum samples. Complex formation method and cloud-point extraction (CPE) coupling with UV-Visible spectrophotometry were used to investigated of study target.The results has showed the best optical characteristic for calibration curve and statistical data which were obtained under optimum conditions. The first method is based on the reaction of MET with nickel (II) in alkaline medium an absorption maximum ?)max) at 434nm. ''Beer's low'' is obeyed in the concentration range (10-100µg.ml-1) with molar absorptivity of 3.9x103 L.mol-1.cm-1.The limit of detection and quantitation values were 2.37 and7.11 µg.ml-1 respectively. The second method based on extraction of traces amounts of MET using the cloud-point extraction (CPE). This method implicated for using of a nonionic surfactant (Triton x-114) as an extraction medium which was entrap the hydrophobic complex formed between MET and nickel(ii) in basic medium as reaction system for designing the CPE procedure. The optimum conditions were similar the first method expect the amount of surfactant which was 0.5 ml. The concentrations range of calibration curve from 3.5to100 µg.ml-1 and molar absorptivity of 1.2x104 L.mol-1.cm-1. In this method was access to less of concentrations in Limit of detection and quantitation which were 0.74and 2.22 µg.ml-1 respectively. The precise (RSD %) and accuracy (recovery %) of both methods were ranged between 0.24-0.47, 97.86-98.68 respectively. The data of two methods were appeared high acceptable with standered of British Pharmacopoeia through using statistic methods (f-test and t-test), that they may be used in analysis of MET.

2015 ◽  
Vol 69 (4) ◽  
Author(s):  
Teodora S. Stefanova ◽  
Kiril K. Simitchiev ◽  
Kiril B. Gavazov

AbstractLiquid-liquid extraction (LLE) and cloud point extraction (CPE) of vanadium(V) ternary complexes with 4-(2-pyridylazo)resorcinol (PAR) and 2,3,5-triphenyl-2H-tetrazolum chloride (TTC) were investigated. The optimal conditions for vanadium extraction and spectrophotometric determination were identified. The composition (V : PAR : TTC) of the extracted species was 1 : 2 : 3 (optimal conditions; LLE), 2 : 2 : 2 (low reagents concentrations; LLE), 1 : 1 : 1 (short heating time; CPE), and 1 : 1 : 1 + 1 : 1 : 0 (optimal extraction conditions; CPE). LLE, performed in the presence of 1,2-diaminocyclohexane-N,N,N’,N’-tetraacetic acid and NH4F as masking agents, afforded the sensitive, selective, precise, and inexpensive spectrophotometric determination of vanadium. The absorption maximum, molar absorptivity, limit of detection, and linear working range were 559 nm, 1.95 × 105 dm3 mol−1 cm−1, 0.7 ng cm−3, and 2.2-510 ng cm−3, respectively. The procedure thus developed was applied to the analysis of drinking waters and steels. The relative standard deviations for V(V) determination were below 9.4 % (4-6 × 10−7 mass %; water samples) and 2.12 % (1-3 mass %; steel samples).


2016 ◽  
Vol 13 (2) ◽  
pp. 426-439
Author(s):  
Baghdad Science Journal

In this study, cloud point extraction combined with molecular spectrometry as an eco-friendly method is used for extraction, enrichment and determination of bendiocarb (BC) insecticide in different complex matrices. The method involved an alkaline hydrolysis of BC followed Emerson reaction in which the resultant phenol is reacted with 4-aminoantipyrene(4-AAP) in the presence of an alkaline oxidant of potassium ferric cyanide to form red colored product which then extracted into micelles of Triton X-114 as a mediated extractant at room temperature. The extracted product in cloud point layer is separated from the aqueous layer by centrifugation for 20 min and dissolved in a minimum amount of a mixture ethanol: water (1:1) followed the determination of BC by using spectrophotometry at a wavelength maximum of 470 nm. The most important parameters affecting the extraction and determination of BC are conducted via a classical optimization. Under the optimum conditions established , Beer’s law is obeyed in the range of 0.1-4 µg mL-1 while the optimum concentration ranges estimated by Ringbom’s plot was of 0.4-2.12 µg mL-1. The enrichment factor was of 59.87 fold leading to achieve the limit of detection of 0.076 ?g mL-1. The proposed method gives superior sensitivity in terms of the molar absorptivity of 1.99x105 L mol-1 cm-1 and extraction efficiency of 98.0%. The established method is applied in the analysis of the spiked vegetables, orange, soil and water samples with appropriate concentration with BC standard.


Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.


2018 ◽  
Vol 5 (4) ◽  
pp. 171500 ◽  
Author(s):  
N. I. Mohd ◽  
N. N. M. Zain ◽  
M. Raoov ◽  
S. Mohamad

A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient ( R 2 ) in the range of 0.991–0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l −1 (atrazine) and 1.22 µg l −1 (propazine), and the limit of quantitation was 3.54 µg l −1 (atrazine) and 4.07 µg l −1 (propazine). Satisfactory recoveries in the range of 81–108% were determined in milk samples at 5 and 1000 µg l −1 , respectively, with low relative standard deviation, n  = 3 of 0.301–7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.


2011 ◽  
Vol 8 (4) ◽  
pp. 1528-1535 ◽  
Author(s):  
F. Nekouei ◽  
Sh. Nekouei

A simple, fast, reproducible and sensitive method for the flotation- spectrophotometric determination of Al3+is reported. The apparent molar absorptivity (ε) of the ion associate was determined to be 8.35×104L mol-1cm-1. The calibration curve was linear in the concentration range of 1.0-50 ng mL-1of Al3+with a correlation coefficient of 0.9997. The limit of detection (LOD) was 0.621 ng mL. The relative standard deviation (RSD) at 10 and 30 ng mL-1of aluminium were 1.580 and 2.410% (n=7) respectively. The method was applied for measuring the amount of aluminium in water samples.


2013 ◽  
Vol 699 ◽  
pp. 34-39
Author(s):  
Li Liu ◽  
Xia Shi Zhu

A new Triton X-114 cloud point extraction combined with fluorometry method for analysis of magnolol in drug samples was developed. Under the optimum conditions, the calibration graph was linear in the range of 2.0-150.0ng/mL of magnolol in the initial solution with r = 0.9998. Detection limit (DL) was 0.03ng/mL (S/N=3) and the relative standard deviation (RSD) for 20.0ng/mL of magnolol was 2.79%(n=11). The method was successfully applied for the determination of magnolol in drug samples with satisfactory results.


2019 ◽  
Vol 16 (2) ◽  
pp. 0332
Author(s):  
Dhahir Et al.

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.


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