scholarly journals Development of Green Method for Trace Determination of Bendiocarb in Real Samples Using Emerson

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):  
Azhar A Ghali ◽  
Ashwoq S Hussein

In this work,Cloud point extraction (CPE) methodology as an one green chemistry method is used for extraction, enrichment and determination ofNi (II) and Cu (II) in the somemedicinal plants,by use organic reagent2-[ (6-Methyl-2-Benzothiazolyl)azo]-4-Chloro Phenol (6-MeBTAClP) for formationthe extracted complexes into micelles of Triton X-114 as a mediated extractant at65,70 C0 respectively. The extracted product in densityhigh (cloud point layer )is separated from the aqueous layer by centrifugation for 15 min and dissolved in 0.5 mLfrom ethanol followed the determination of Ni (II) and Cu (II)by using spectrophotometry at a wavelength maximum of 644 and 598 nm respectively. The optimum conditions established as pH, The linear range of Ni (II) and Cu (II)along with limit of detection,precision expressed as relative standard deviation for seven replication measurements and the recovery range were obtained for Ni (II) and Cu (II) ions,respectively. The complex s identified by UV-Visible and IR spectra. The mole ratio method and continuous variation method (Job’s method)also investigated.


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.


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.


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.


2021 ◽  
Vol 33 (10) ◽  
pp. 2472-2476
Author(s):  
Rajib Joarder

A simple, sensitive, quick, easy and efficient (SSQuEE) analytical technique based on cloud point extraction (CPE) has been developed for the determination of different pesticides present in soil and water with high performance liquid chromatography separation and ultraviolet detection. The environmentally friendliness surfactant like Triton X -100, compared to Tween series of non-ionic surfactant can effectively extract imidacloprid (insecticide), flusilazole (fungicide) and atrazine (herbicide) at cloud point temperature at 67 ºC, 82 ºC and 62 ºC, respectively. To reach the optimum extraction efficiency, different experimental parameters like surfactant concentration, salt type and its concentration, equilibrium time and temperature, pH were observed. At the optimum conditions, linear regression coefficient of the standard curves was greater than 0.9924. The limit of detection of imidacloprid, flusilazole and atrazine were 0.10 μg L-1, 0.24 μg L-1, 0.15 μg L-1 and recovery percent are 99.71 %, 88.1% and 89.74%, respectively.


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).


2018 ◽  
Vol 39 (4) ◽  
pp. 65
Author(s):  
K. B. Vinay ◽  
H. D. Revanasiddappa ◽  
M. R. Divya ◽  
N. Rajendraprasad

Three simple and sensitive spectrophotometric methods are described for the determination of ofloxacin (OFX) in pharmaceuticals and in spiked human urine. First and second methods are based on the measurement of absorbance of OFX in 0.1 M HCl at 293 nm (method A) and 0.1 M NaOH at 287 nm, respectively. The third method is based on the measurement of2:1 complex formed between OFX and iron(III) in H2SO4 medium, the complex peaking at 420 nm (method C). The optimum conditions for all the three methods are optimized. Beer’s lawis obeyed over the ranges 0.63-12.5 using method A and method B, and 10-120 μg mL-1 using method C. The apparent molar absorptivity values are calculated to be 3.5 × 104, 2.76 × 104 and2.51 × 103 L mol-1cm-1 for method A, method B and method C, respectively. The Sandell sensitivity, limit of detection (LOD) and limit quantification (LOQ) values are also reported. All the methods were validated in accordance with current ICH guidelines. The developed methods were employed with high degree of precision and accuracy for the estimation of total drug content in commercial tablet formulations of DOX. The results obtained from human spiked urine are satisfactory and recovery values are in the range 95.5-106.6%.


2020 ◽  
Vol 17 (35) ◽  
pp. 628-639
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Raghad Saad HATAM ◽  
Ahmed F. KUDHAIR ◽  
Noor Jamal MOHAMMED

The simple, rapid, economical, and environmentally friendly method was developed for spectrophotometric determination of ranitidine hydrochloride (R-HCl) in pharmaceutical samples after extraction by the cloud point method. The method based on the reduction of Fe(III) by ranitidine hydrochloride to Fe(II), which subsequently reacted with ferricyanide to form colored products at (pH 4.0), then Triton X–114 surfactant was used as an extractant for ranitidine hydrochloride. The linearity of the calibration curve was maintained from concentrations between 0.5–60.0 μg/mL at the maximum absorption 693 nm. Factors required for reaction conditions including pH, FeCl3, and K3[Fe(CN)6] concentration, the volume of surfactant, temperature, time, and order of addition were investigated. Regression analysis indicates that the correlation coefficient was 0.9998 and the molar absorptivity was 0.46x104 L/mol.cm. Detection and quantification limits were 0.475 and 1.567 μg/mL, respectively. The confidence limit of slope and the confidence limit of the intercept at 95% were 0.0147 ± 0.00015 and 0.0642 ± 0.01033. Sandell`s sensitivity was also calculated and it was found 0.0680 μg/cm2. The preconcentration factor was 50.0%. Validation studies for three different concentrations (5.0, 10.0 and 30.0) μg/mL of ranitidine hydrochloride gave relative standard deviations between 0.142–0.728 and the percentage recoveries ranged from 98.780 ± 0.719 – 99.840 ± 0.142. The proposed method was successfully applied for the determination of ranitidine hydrochloride in some of its pharmaceutical products with recovery between 99.108–99.808 and RSD% between 0.012–0.031. The results obtained from the proposed method make it suitable to use in the determination of ranitidine hydrochloride in its bulk and tablet dosage form.


2020 ◽  
Vol 85 (1) ◽  
pp. 89-96 ◽  
Author(s):  
Denys Snigur ◽  
Alexander Chebotarev ◽  
Vitaliy Dubovyi ◽  
Dmytro Barbalat ◽  
Anastasiia Klochkova

The novel cloud point extraction procedure for preconcentration of copper(II) was discovered. A simple chemical method for initiating the cloud point extraction (CPE) has been proposed. The formation of surfactant rich phase in a system containing a nonionic surfactant Triton X-100, copper(II), 6,7-dihydroxy-4-methyl-2-phenylbenzopyrilium chloride (DHMPhB) and ammonium benzoate is observed immediately upon the sulfuric acid addition into solution. Under the optimal conditions (absorption band maximum was 540 nm, concentration 1.5?10-4 mol dm-3 of DHMPhB, 1.0 vol.% of Triton X-100, 2.0 cm3 of 0.75 mol dm-3 ammonium benzoate, and 1.0 cm3 of 0.5 mol dm-3 sulfuric acid solution for obtaining benzoic?benzoate buffer solution with pH 4.5 and initiation immediate surfactant rich phase formation) the calibration plot for spectrophotometric determination of copper(II) was linear in the range of copper(II) concentration 0.02?0.95 ?g cm?3. The limit of detection was calculated 0.006 ?g cm?3. The water samples were analyzed according to a suggested procedure with satisfactory results.


2020 ◽  
Vol 17 (3) ◽  
pp. 0780
Author(s):  
Takleef Sallal ◽  
Sumayha Abbas

Rapid, reproducible and accurate method has been developed for the assay for of mebendazol (MBZ) residual assay. The method is based on alkaline hydrolysis of MBZ with sodium hydroxide then oxidation with N-bromosuccinimide (NBS) followed by coupling with 4-Bromoaniline (4-BA) to yield a highly colored product absorbed at maximum 434 nm. Regression analysis of linearity range was found (0.6-2.8) µg.ml-1.  The optimum conditions that affect the oxidation were studied. The developed method was found to be precise with mean value of relative standard deviation (1.153- 1.303) and accurate with relative error (-0.5940-1.7821) .The calculated molar absorptivity and sandal sensitivity values of (29825 L.mol-1.cm-1), 0.0099 µg.cm-2 respectively.  The limit of detection and limit of quantitation were of 0.04696, 0.156548 µg.ml-1 respectively .The suggested method showed good recovery with a mean value of 100.77% for analysis of dosage forms.


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