scholarly journals TITRIMETRIC AND SPECTROPHOTOMETRIC ASSAY OF BUPROPION HYDROCHLORIDE IN PHARMACEUTICALS USING MERCURY(II) NITRATE

2018 ◽  
Vol 35 (3) ◽  
pp. 09
Author(s):  
M. A. Sameer Abdulaziz ◽  
K. Basavaiah ◽  
K. B. Vinay

Two simple, rapid and accurate methods for the determination of bupropion hydrochloride (BUP) in pure and in pharmaceutical preparations are described. Both methods are based on the measurement of the chloride of its hydrochloride. In the titrimetric method, the chloride content of bupropion hydrochloride is determined by titrating with mercury(II)nitrate using diphenylcarbazone–bromophenol blue as indicator. Titrimetric method is applicable over a range 2–20 mg of BUP and the reaction stoichiometry is found to be 2:1 (BUP: Hg(NO3)2).The spectrophotometric method involves the addition of a measured excess of mercury(II) nitrate reagent in formate buffer to the drug, and after ensuring the reaction had gone to completion, the unreacted mercury(II) is treated with a fixed amount of diphenylcarbazone, and absorbance measured at 515 nm. The absorbance is found to decrease linearly with increasing concentration of BUP and the calibration curve is linear over 1.0–15.0 μg mL–1 BUP. The proposed methods were successfully applied to the determination of BUP in commerciallyavailable dosage forms with good accuracy and precision, and without  detectable interference by excipients. The accuracy was further ascertained by placebo blank and synthetic mixture analyses and also by recovery experiments via standard-addition procedure.

2013 ◽  
Vol 19 (1) ◽  
pp. 121-128 ◽  
Author(s):  
Hemavathi Deepakumari ◽  
Shiramahally Mallegowda ◽  
Kanakapura Vinay ◽  
Hosakere Revanasiddappa

Two simple, sensitive and extraction-free spectrophotometric methods are described for the estimation of risperidone (RSP) in both pure and in pharmaceutical preparations. The proposed methods are based on the formation of ion-pair complex between RSP and the dyes, bromophenol blue (BPB) in method A and Phenol red (PR) in method B at room temperature to form yellow colored products which show maximum absorbance at 410 and at 400 nm in methods A and B, respectively. Beer's law was obeyed in the concentration range of 0.5-10 and 0.5-25 ?g mL-1 in methods A and B with apparent molar absorptivities of 3.43 ? 104 and 0.85 ? 104 L moL-1 cm-1, respectively. The limit of detection for method A is found to be 0.0056 and for method B is 0.132 ?g mL-1. The composition of the ion-pairs was established by Job?s method and it was found to be 1:1 for both the methods A and B. The proposed methods have been applied successfully to the determination of RSP in pharmaceutical preparations. The results were statistically compared with those of a reference method by applying the Student?s t-test and F-test. The methods developed were validated for accuracy and precision by performing recovery experiments via standard addition technique.


2007 ◽  
Vol 90 (1) ◽  
pp. 102-112 ◽  
Author(s):  
Yasser Shaker El-Saharty ◽  
Fadia H Metwally ◽  
Mohamed Refaat ◽  
Sonia Zaki El-Khateeb

Abstract A binary mixture of hyoscine butylbromide and ketoprofen was determined by 4 different methods. The first involved determination of hyoscine butylbromide and ketoprofen using the ratio-spectra first-derivative spectrophotometric technique at 211 and 234 nm over the concentration ranges of 2-14 and 5-45 μg/mL with mean accuracies 99.84 ± 0.92 and 99.98 ± 0.64%, respectively. The second method utilized second-derivative spectrophotometry over the concentration ranges of 2-14 and 5-35 μg/mL with mean accuracies 99.32 ± 1.06 and 99.55 ± 1.15%, respectively. The third method was based on the resolution of the 2 components by bivariate calibration depending on a simple and rapid mathematical algorithm and quantitative evaluation of the absorbances at 206 and 254 nm over concentration ranges of 2-16 and 5-35 μg/mL; mean accuracies of 100.21 ± 1.30 and 100.19 ± 1.07% were obtained for hyoscine butylbromide and ketoprofen, respectively. The fourth method was reversed-phase liquid chromatography using 0.05 M ammonium dihydrogen phosphateacetonitrilemethanol (20 + 30 + 6, v/v) as the mobile phase with ultraviolet detection at 220 nm over concentration ranges of 1-90 and 5-70 μg/mL; mean accuracies were 99.92 ± 1.02 and 99.61 ± 0.98%, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical preparations. The methods retained their accuracy and precision when the standard addition technique was applied. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.


2014 ◽  
Vol 1033-1034 ◽  
pp. 521-525
Author(s):  
Cheng Ying Zhou ◽  
Wei Qu ◽  
Liu Lu Cai

This paper determined the total absorbance of phosphorus molybdenum blue and arsenic molybdenum blue by using the additive property of their absorbance values. By eliminating the interference of arsenic by reduction masking with composite reducing agent Na2SO3-Na2S2O3-KBr, the absorbance of phosphorus could be obtained. Thus, the content of phosphorus and arsenic could be calculated, respectively. The results show that the work curves of this method for phosphorus and arsenic are consistent with Beer’s law when the content of phosphorus and arsenic is 0-0.60ug/mL and 0-2.00ug/mL, respectively. The standard addition recovery rate of phosphorus and arsenic is 98.80%-101.04% and 99.00%-101.50%, respectively. The relative standard deviation of phosphorus and arsenic is less than 4.0% with good accuracy and precision. This method is simple and fast to determine phosphorus and arsenic in molybdenum concentrate, and the results are accurate and reliable.


2020 ◽  
Vol 10 (02) ◽  
pp. 311-317
Author(s):  
Yusur Q. Ismaeel ◽  
Bashaer A. Al-Phalahy

New, simple, sensitive and rapid method for the determination of propranolol in the pharmaceutical preparations and human fluids. The Buildup and electrochemical response characteristics of a poly vinyl chloride (PVC) selective membrane electrode for the determination of propranolol (POP) are described in this research. The proposed electrodes was composed of propranolol-bromophenol blue as ion-exchanger and Di-butyl phthalate (DBPH) (electrode A), tris (2-ethylhexyl) phosphate (TEHP) (electrode B), and ortho-nitrophenyloctylether (ONPOE) (electrode C), as plasticizers. The slope was 50.94, 57.77, and 49.75 mV/decade for electrode A, B and C. the linear range was 5 ×10-5 – 1×10-2, 1×10-4 – 1×10-2, and 5×10-5 – 1×10-2 M, a detection limit of 4.2×10-5, 8.9×10-5, and 4.8×10-5 M, lifetime of 21, 42, and 1-day, respectively. Electrode B gives the best results, so the application of pharmaceutical and human fluids was based upon this electrode, the recovery percentage was 103, 101, 102.5, and 104 for POP tablet 10mg, tablet 40mg, urine and plasma by standard addition method, respectively.


2011 ◽  
Vol 47 (2) ◽  
pp. 251-260 ◽  
Author(s):  
Kanakapura Basavaiah Vinay ◽  
Hosakere Doddarevanna Revanasiddappa ◽  
Okram Zenita Devi ◽  
Pavagada Jagannathamurthy Ramesh ◽  
Kanakapura Basavaiah

One titrimetric and two spectrophotometric methods have been described for the determination of ofloxacin (OFX) in bulk drug and in tablets, employing N-Bromosuccinimide as an analytical reagent. The proposed methods involve the addition of a known excess of NBS to OFX in acid medium, followed by determination of unreacted NBS. In titrimetry, the unreacted NBS is determined iodometrically, and in spectrophotometry, unreacted NBS is determined by reacting with a fixed amount of either indigo carmine (Method A) or metanil yellow (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of OFX. Titrimetry allows the determination of 1-8 mg of OFX and the calculations are based on a 1:5 (OFX:NBS) reaction stoichiometry. In spectrophotometry, Beer's law is obeyed in the concentration ranges 0.5-5.0 µg/mL for method A and 0.3-3.0 µg/mL for method B. The molar absorptivities are calculated to be 5.53x10(4) and 9.24x10(4) L/mol/cm for method A and method B, respectively. The methods developed were applied to the assay of OFX in tablets, and results compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via the standard-addition method.


2003 ◽  
Vol 71 (3) ◽  
pp. 179-194
Author(s):  
W. El-Hawary ◽  
A. Shoukry ◽  
A. Talat

The interaction of hydralazine hydrochloride with picric acid (I), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) (II), 2,4-dinitrobenzoic acid (III), bromanil (IV) and chloranil (V) was found to be useful for its spectrophotometric determination. The determination was carried out at 520, 510, 550, 540 and 535 nm for the reaction with (I), (II), (III), (IV) and (V), respectively. The effect of several variables on the colouring process was studied. The proposed methods have been applied successfully for the determination of hydralazine hydrochloride in pure samples and in pharmaceutical preparations with good accuracy and precision. The results were compared to those obtained by the official and pharmacopoeia1 methods. The linear ranges for obedience of Beer's law are up to 118, 54,639, 27.5 and 78.6 mg/l, Ringbom ranges are 13-100, 7.6-44.7, 77.4-445.0, 5.8-25.8 and 22.5-63.1 μg/ml, Detection limits are 4.8, 2.2, 18.4, 1.2 and 5.9 mg/l, and RSD 0.042, 0.037, 0.043, 0.013 and 0.073 for reactions of hydralazine hydrochloride with I, II, III, IV and V, respectively.


2002 ◽  
Vol 70 (1) ◽  
pp. 49-55
Author(s):  
Abou-Attia Fekria M. ◽  
Issa Y.M. ◽  
El Reis M.A. ◽  
Aly F.A. ◽  
Abd El- MoetY M.

The formation of the azo-dye using chromotropic acid as a coupling agent was applied to the determination of five sulphonamides. The spectrophotometric studies as well as microanalysis of the studied sulphonamides- chromotropic acid azo dyes revealed the existence of the 1:1 coupling product. The absorbance of the formed azo dye is measured at 510 nrn, and has a large molar absorptivity (ε = 2.87 - 3.29 × 104 1 mol−1cm−1). Beer's law was obeyed over the concentration range 0.5-9.0 µg ml−1. The assay results of pharmaceutical formulations showed good accuracy and precision over the concentration range used. The proposed method avoids time-consumption, extraction process and temperature control.


2011 ◽  
Vol 17 (1) ◽  
pp. 81-89 ◽  
Author(s):  
Zenita Devi ◽  
K. Basavaiah ◽  
K.B. Vinay

Three simple and sensitive spectrophotometric methods are described for the determination of domperidone (DOM) in bulk drug and in dosage forms using bromate-bromide mixture as brominating agent in acid medium and three dyes, meta-cresol purple (MCP), amaranth (AMR) and erioglaucine (EGC). The methods involve the addition of a known excess of bromate-bromide mixture to an acidified solution of DOM followed by the determination of the residual bromine by reacting with a fixed amount of either MCP dye and measuring the absorbance at 530 nm (method A) or AMR dye and measuring the absorbance at 520 nm (method B) or EGC dye and measuring the absorbance at 630 nm (method C). Beer?s law is obeyed over the concentration ranges, 0.63 - 10.0, 0.25-4.0 and 0.13-2.0 ?g mL-1 for method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 3.751 ? 104, 6.604 ? 104 and 1.987 ? 105 L mol-1cm-1 for method A, method B and method C, respectively and the corresponding sandell sensitivity values are 0.011, 0.006 and 0.002 ?g cm-2. The limit of detection and the limit of quantification are also reported for all the three methods. No interference was observed from common additives found in pharmaceutical preparations. Statistical comparisons of the results with those of the reference method showed an excellent agreement, and indicated no significant difference in accuracy and precision. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition technique.


2010 ◽  
Vol 93 (3) ◽  
pp. 904-910 ◽  
Author(s):  
Sejal K Patel ◽  
Natvarlal J Patel

Abstract A binary mixture of imipramine HCl and chlordiazepoxide was determined by three different methods. The first involved determination of imipramine HCl and chlordiazepoxide using the first derivative spectrophotometric technique at 219 and 231.5 nm over the concentration ranges of 120 and 224 g/mL with mean accuracies of 99.47 0.78 and 101.43 1.20, respectively. The second method utilized RP-HPLC with methanolacetonitrile0.065 M ammonium acetate buffer (45 + 25 + 30, v/v/v, pH adjusted to 5.6 0.02 with phosphoric acid) as the mobile phase pumped at a flow rate of 1.0 mL/min. Quantification was achieved using UV detection at 240 nm over concentration ranges of 0.254.0 and 0.11.6 g/mL, with mean accuracies of 101.17 0.56 and 100.67 0.40 for imipramine HCl and chlordiazepoxide, respectively. The third method was HPTLC with carbon tetrachlorideacetonetriethylamine (pH 8.3; 6 + 3 + 0.3, v/v/v) as the mobile phase. Quantification was achieved with UV detection at 240 nm over concentration ranges of 50600 and 20240 ng/spot with mean accuracies of 99.51 0.59 and 100.59 0.84 for imipramine HCl and chlordiazepoxide, respectively. The suggested procedures were checked using prepared mixtures, and were successfully applied for the analysis of pharmaceutical preparations. The accuracy and precision of the methods were confirmed when the standard addition technique was applied. The results obtained by applying the proposed methods were statistically analyzed.


2007 ◽  
Vol 4 (1) ◽  
pp. 117-127 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar

One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT) in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS) as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involves adding a measured excess of NBS to MPT in acid medium followed by determination of residual NBS by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (Method A) or indigo carmine and measuring the absorbance at 610 nm (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of MPT. Reaction conditions have been optimized. Titrimetry allows the determination of 1 - 12 mg of MPT and the calculations are based on a 1: 4 (MPT: NBS) reaction stoichiometry. In spectrophotometry, the measured absorbance is found to increase linearly with the concentration of MPT serving as basis for quantitation. The systems obey Beer’s law for 0.5 - 4.0 μg mL-1and 1.25 - 10.0 μg mL-1for method A and method B, respectively. The apparent absorptivities are calculated to 1.07 × 105be and 4.22 × 104L mol cm-1for method A and method B, respectively. The methods developed were applied to the assay of MPT in commercial tablet formulations, and the results were compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition method.


Sign in / Sign up

Export Citation Format

Share Document