Cloud Point Extraction and Spectrophotometry Determination of Lead in Environment Water Using 5-Br-PADAP

2013 ◽  
Vol 830 ◽  
pp. 345-348
Author(s):  
Lin Gao ◽  
Sheng Jie Chen ◽  
Fang Chen ◽  
Wen Hong Zhou ◽  
Jun Long Yao

A simple, sensitive, green and low cost detection method based on the cloud point extraction (CPE) separation and spectrophotometry was proposed for the determination of lead. In pH=9.0 H3BO3 buffer solution, Pb(II) reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) in the presence of Triton X-100 yielding a hydrophobic complex, which then is extracted into micro-volume surfactant-rich phase. The calibration graph was linear in the range of 20-400 µg/L (at 560 nm). Under the optimized conditions, the detection limits of 10.94 µg/L and the relative standard deviations(RSD) of 2.0% (n=5) for Lead(II) were found, respectively. The sensitivity and absorbance of this method are at least five times higher when compared with that of usual 5-Br-PADAP spectrophotometry without CPE, and the proposed method has been applied to the determination of Lead in environment water samples with satisfactory results.

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.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Mohammad Hosein Soruraddin ◽  
Rouhollah Heydari ◽  
Morteza Puladvand ◽  
Mir Mehdi Zahedi

A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL-1; the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL-1of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.


2020 ◽  
Vol 17 (1) ◽  
pp. 0057
Author(s):  
Maha Al-Tameemi

In current article an easy and selective method is proposed for spectrophotometric estimation of metoclopramide (MCP) in pharmaceutical preparations using cloud point extraction (CPE) procedure. The method involved reaction between MCP with 1-Naphthol in alkali conditions using Triton X-114 to form a stable dark purple dye. The Beer’s law limit in the range 0.34-9 μg mL-1 of MCP with r =0.9959 (n=3) after optimization. The relative standard deviation (RSD) and percentage recoveries were 0.89 %, and (96.99–104.11%) respectively. As well, using surfactant cloud point extraction as a method to extract MCP was reinforced the extinction coefficient(ε) to 1.7333×105L/mol.cm in surfactant-rich phase. The small volume of organic solvent (500mL/sample) provides an environmentally friendly and low-cost preconcentration method. The suggested method was utilized for analyzing of MCP in commercial pharmaceutical injections.


2019 ◽  
Vol 16 (1) ◽  
pp. 41 ◽  
Author(s):  
Nurul Azwa Mohd Azizi ◽  
Nurul Yani Rahim ◽  
Muggundha Raoov Ramachandran ◽  
Saliza Asman

The cloud point extraction (CPE) method was developed to determine the zinc prior to Ultraviolet-visible (UV-Vis) spectrophotometry detection. Triton X-100 was applied as extractant based on the complexation reaction of Zn(II) ions with ethylenediaminetetraacetic acid (EDTA). Under optimal conditions, the CPE was used to determine the concentration of zinc in canned food samples. The amounts of zinc found in the food samples were in the range of 0.005-0.007 mg/L with relative standard deviation (RSD) of < 8 %. This confirmed that the proposed CPE method is suitable for the determination of zinc in food samples, indicating the concentration of zinc was within the permissible limit.


2021 ◽  
pp. 174751982110273
Author(s):  
Quan Han ◽  
Yanyan Huo ◽  
Xiaohui Yang ◽  
Xing Yao

A highly sensitive method for the determination of ultra-trace levels of palladium in water samples by cloud point extraction and graphite furnace atomic absorption spectrometry is developed. The procedure is based on complexation of palladium with a laboratory-prepared novel chelating agent, 2-(5-bromo-4-methyl-2-pyridylazo)-5-dimethylaminoaniline (5-Br-4-CH3-PADMA) and subsequent micelle-mediated extraction of the product using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) as an extracting agent. Analytical parameters affecting the separation and detection process, such as pH, concentration of the chelating agent and surfactant, equilibration temperature, and time are investigated. The optimized conditions are as follows: pH 6.0 HAc–NaAc buffer solution, 1 × 10−5 mol L−1 5-Br-4-CH3-PADMA, and 0.1% (w/v) Triton X-114. Under the optimized conditions, the calibration graph is linear in the range of 0.1–12 ng/mL, the detection limit is 0.05 ng/mL for palladium, and the relative standard deviation is 2.9% ( c = 1.0 ng/mL, n = 10). The enrichment factor, defined as the ratio of the aqueous solution volume to that of the surfactant-rich phase volume after dilution with HNO3–methanol solution, is 200. The proposed method is applied to the determination of palladium in water samples with satisfactory results.


RSC Advances ◽  
2016 ◽  
Vol 6 (77) ◽  
pp. 73797-73804
Author(s):  
Alaa S. Amin ◽  
Mohammed A. Kassem ◽  
Sayed M. N. Moalla

Effect of 5.0% Triton X-100 on the complexation of 40 ng mL−1 Sc(iii) with ATAP.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Mohammad Reza Jamali ◽  
Mohammad Gholinezhad ◽  
Saiedeh Balarostaghi ◽  
Reyhaneh Rahnama ◽  
Seyed Hojjat Allah Rahimi

A new, simple, and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of cobalt. The cobalt ions in the initial aqueous solution were complexed with 4-Benzylpiperidinedithiocarbamate, and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the cobalt content was measured by flame atomic absorption spectrometry. The main factors affecting CPE procedure, such as pH, concentration of ligand, amount of Triton X-114, equilibrium temperature, and incubation time were investigated and optimized. Under the optimal conditions, the limit of detection (LOD) for cobalt was 0.5 μg L-1, with sensitivity enhancement factor (EF) of 67. Calibration curve was linear in the range of 2–150 μg L-1, and relative standard deviation was 3.2% (c=100 μg L-1;n=10). The proposed method was applied to the determination of trace cobalt in real water samples with satisfactory analytical results.


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.


2020 ◽  
Vol 13 (12) ◽  
pp. 458
Author(s):  
Elżbieta Gniazdowska ◽  
Natalia Korytowska ◽  
Grzegorz Kłudka ◽  
Joanna Giebułtowicz

Cloud-point extraction (CPE) is rarely combined with liquid chromatography coupled to mass spectrometry (LC–MS) in drug determination due to the matrix effect (ME). However, we have recently shown that ME is not a limiting factor in CPE. Low extraction efficiency may be improved by salt addition, but none of the salts used in CPE are suitable for LC–MS. It is the first time that the influences of a volatile salt—ammonium acetate (AA)—on the CPE extraction efficiency and ME have been studied. Our modification of CPE included also the use of ethanol instead of acetonitrile to reduce the sample viscosity and make the method more environmentally friendly. We developed and validated CPE–LC–MS for the simultaneous determination of 21 antidepressants in plasma that can be useful for clinical and forensic toxicology. The selected parameters included Triton X-114 concentration (1.5 and 6%, w/v), concentration of AA (0, 10, 20 and 30%, w/v), and pH (3.5, 6.8 and 10.2). The addition of 10% of AA increased recovery twice. For 20 and 30% (w/v) of AA, three phases were formed that prolonged the extraction process. The developed CPE method (6% Triton X-114, 10% AA, pH 10.2) was successfully validated through LC–MS/MS simultaneous determination of 21 antidepressants in human plasma. The linearity was in the range of 10–750 ng/mL (r2 > 0.990).


2011 ◽  
Vol 6 ◽  
pp. ACI.S5949 ◽  
Author(s):  
Sabah Shiri ◽  
Ali Delpisheh ◽  
Ali Haeri ◽  
Abdolhossein Poornajaf ◽  
Tahereh Khezeli ◽  
...  

A novel and sensitive floatation-spectrophotometric method is presented for determination of trace amounts of thorium in water samples. The method is based on the ion-associated formation between thorium, Eriochrome cyanine R and Brij-35 at pH = 4 media. The complex was floated in the interface of the aqueous phase and n-hexane by vigorous shaking. After removing the aqueous phase the floated particles were dissolved in methanol and the absorbance was measured at 607 nm. The influence of different important parameters such as Eriochrome cyanine R and surfactants concentration, pH, volume of n-hexane, standing time and interfering ions were evaluated. Under optimized conditions the calibration graph was linear in the range of 6-230 ng mL-1 of thorium with a correlation coefficient of 0.9985. The limit of detections (LOD), based on signal to noise ratio (S/N) of 3 was 1.7 ng mL-1. The relative standard deviations for determination of 150 and 30 ng ml-1 of thorium were 3.26 and 4.41%, respectively (n = 10). The method showed a good linearity, recoveries, as well as some advantages such as sensitivity, simplicity, affordability and a high feasibility. The method was successfully applied to determine thorium in different water and urine samples.


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