Spectrophotometric determination of astemizole

Four simple and sensitive spectrophotometric methods for the determination of astemizole (AZ) in pure samples and pharmaceutical formulations are described. They are based on the oxidation of astemizole with excess N-bormosuccinimide (NBS) and determination of the unconsumed NBS with, metol-sulphanilamide (method A, lambda(max): 520 nm) or celestine blue (method B, lambda(max): 540 nm); or by the reduction of Folin-ciocalteu reagent (method C, lambda(max): 720 nm); or by the formation of a chloroform-soluble, coloured ion-association complex between the drug and azocarmine G (AG) at pH 1.5 (method D, lambda(max); 540 nm). The results obtained are reproducible with a coefficient of variation of less than 1.0%.     

Determination of doxorubicin hydrochloride by visible spectrophotometry

Four simple and sensitive visible spectrophotometric methods (A-D) have been described for the assay of doxorubicin hydrochloride either in pure form or in pharmaceutical formulations. Method A was developed based on oxidation of the drug with Fe(III) to produce Fe(II), which subsequently reacts with 1.10-ortho-phenanthroline to form a red colored complex (lambda(max): 510 nm) at pH 4.6. Method B involves the reduction of Folin-Ciocalteu (F-C) reagent by the drug and the reduced species formed possesses a characteristic intense blue color (lambda(max): 770 nm). In methods C and D. oxidation of the drug with periodate at specified experimental conditions yields formaldehyde and dialdehyde, which in turn react either with 3-methyl-2-benzothiazolinone hydrazone hydrochloride to form an intensely brilliant blue cationic dye (lambda(max): 620-670 nm. method C) or by condensation with phenylhydrazine hydrochloride (PHH) to form orange-red colored product (lambda(max): 510 nm, method D) in the presence of potassium ferricyanide. All of the variables have been optimized and the reaction mechanisms presented. The concentration measurements are reproducible within a relative standard deviation of 1.0%.     

Three simple spectrophotometric methods for the determination of sulphinpyrazone

Three simple and sensitive spectrophotometric methods for the determination of sulphinpyrazone (SP) in bulk samples and pharmaceutical formulations are described. They are based on the oxidation of sulphinpyrazone with excess N-bromosuccinimide (NBS) and determination of the unconsumed NBS with metol-isonicotinic acid hydrazide (method A, lambda(max): 620 nm); by the reduction of Folin-Ciocalteu reagent (method B, lambda(max) 770 nm); or by the formation of a chloroform-soluble, coloured ion-association complex between the drug and Methylene Violet (MV) at pH 7.0 (method C, lambda(max) 545 nm).     

Utility of oxidation-reduction reaction for the determination of ranitidine hydrochloride in pure form,in dosage forms and in the presence of its oxidative degradates

Three simple, accurate and sensitive colorimetric methods (A, B and C) for the determination of ranitidine HCl (RHCl) in bulk sample, in dosage forms and in the presence of its oxidative degradates are described. The first method A is based on the oxidation of the drug by N-bromosuccinimide (NBS) and determination of the unreacted NBS by measurement of the decrease in absorbance of amaranth dye (AM) at a suitable lambda(max)=520 nm. The methods B and C involve the addition of excess Ce(4+) and determination of the unreacted oxidant by decrease the red color of chromotrope 2R (C2R) at a suitable lambda(max)=528 nm for method B or decrease the orange pink color of rhodamine 6G (Rh6G) at a suitable lambda(max)=526 nm for method C. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 0.2-3.6, 0.1-2.8 and 0.1-2.6 microg ml(-1) for methods A, B and C, respectively. The apparent molar absorptivity. Sandell sensitivity, detection and quantitation limits were calculated. For more accurate results, Ringbom optimum concentration ranges were 0.3-3.4, 0.2-2.6 and 0.2-2.4 microg ml(-1) for methods A, B and C, respectively. Analyzing pure and dosage forms containing RHCl tested the validity of the proposed methods. The relative standard deviations were 相似文献   

Spectrophotometric methods for the determination of labetalol hydrochloride in pure and dosage forms

Simple and sensitive Spectrophotometric methods for the determination of labetalol hydrochloride are described. The first two are based on the oxidative coupling reaction of labetalol hydrochloride withp-N,N-dimethyl-phenylenediamine dihydrochloride (method A, _max 685 nm) and 3-methyl-2-benzothiazolinone hydrazone hydrochloride (method B, _max 545 nm) in the presence of sodium hypochlorite and eerie ammonium sulphate as oxidants, respectively. The third depends on the formation of an ion-association complex of labetalol hydrochloride with suprachen violet 3B at pH 1.3, which is extracted into chloroform (method C, _max 565 nm). The methods obey Beer's law and the precision and accuracy of the methods were checked against the B.P. reference method and the relative standard deviations were in the range 0.35–0.52%. These methods are applied to the determination of labetalol in dosage forms.     

Spectrophotometric methods for the determination of omeprazole in bulk form and pharmaceutical formulations

Four simple and sensitive methods for the assay of omeprazole (OMZ) were developed. These methods are based on the formation of colored species by treating OMZ with 3-methyl-2-benzothiazolinone hydrazone (MBTH) following oxidation with ferric chloride (method A) or m-aminophenol following oxidation with chloramine-T (CAT) (method B) or Folin-Ciocalteau reagent (FC) (method D), or by oxidizing OMZ with excess N-bromosuccinimide (NBS) and determining the consumed NBS with a decrease in color intensity of Celestine blue (CB) (method C). All variables have been optimized. Regression analysis of Beer's plots showed good correlation in the concentration range of 1.0-10, 2.0-32, 0.4-2.4 and 0.8-10 mug ml(-1) for methods A, B, C and D, respectively. No interference was observed for formulation additives and the validity of each method was tested by analysing capsules containing OMZ. Recoveries were 98.7-100.1%.     

Spectrophotometric methods for the determination of anti-emetic drugs in bulk and in pharmaceutical preparations.

Four rapid, simple, reproducible and sensitive methods (A-D) for assaying domperidone (I) and metoclopramide (II) in a bulk sample and in dosage forms were investigated. The first and second methods, A and B, are based on the oxidation of I and/or II by Fe3+ in the presence of o-phenanthroline (o-phen) or bipyridyl (bipy). The formation of tris-complex upon reactions with Fe3+-o-phen and/or Fe3+-bipy mixture in an acetate buffer solution of the optimum pH-values was demonstrated. Methods C and D involve the addition of excess Ce4+ and the determination of unreacted oxidant by a decrease of the red color of chromotrope 2R (C2R) at a suitable lambda(max) of 528 nm for method C, or a decrease in the orange pink color of Rhodamine 6G (Rh6G) at a suitable lambda(max) value of 525 nm for method D. A regression analysis of Beer-Lambert plots showed a good correlation in the concentration range of 0.2-5.8 microg ml(-1). The apparent molar absorptivity, Sandell sensitivity, detection and quantification limits were calculated. For a more accurate analysis, the Ringbom optimum concentration ranges are 0.35-5.6 microg ml(-1). The developed methods were successfully applied to the determination of domperidone and metoclopramide in bulk and pharmaceutical preparations without any interference from common excipients.     

A rapid spectrophotometric assay of some organophosphorus pesticide residues in vegetable samples

A rapid and sensitive spectrophotometric method for the determination of some organophosphorus insecticides, i.e. malathion, dimethoate and phorate is described. It is based on the oxidation of organophosphorus pesticide with slight excess of N-bromosuccinimide (NBS) and the unconsumed NBS is determined with rhodamine B (lambda max: 550 nm). Beer's law is obeyed in the concentration range 0.108-1.08, 0.056-0.56 and 0.028-0.28 microg mL(-1) for malathion, phorate and dimethoate, respectively. The method has been successfully applied for the determination of organophosphorus pesticide residues in various vegetable samples.     

Spectrophotometric estimation of ketotifen fumarate in pharmaceutical formulations

Four simple and sensitive spectrophotometric methods (A–D) for the determination of Ketotifen fumarate in bulk samples and pharmaceutical formulations are described. They are based on the formation of coloured species by the coupling of the diazotised sulphanilamide with the drug (method A, _max 520 nm) or by oxidizing it with excessN-bromo-succinimide and determining the consumed NBS with decrease in colour intensity of celestine blue (method B: _max 540 nm) or by the reduction of Folin-Ciocalteau reagent (method C: _max 720 nm) or by the formation of a chloroform-soluble, coloured ionassociation complex between the drug and Azocarmine G at pH 1.5 (method D: _max 540 nm). Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 1–10, 2–12, 4–28 and 2.5–25 g/ml for methods A–D, respectively. The validity of the proposed methods was tested by analysing pharmaceutical formulations containing KTF: the relative standard deviations were within ±1.0%. Recoveries were 98.9–100.2%.     

Spectrophotometric methods for the determination of certain catecholamine derivatives in pharmaceutical preparations

Two simple, rapid and sensitive spectrophotometric methods for the determination of catecholamine derivatives (pyrocatechol, dopamine, levodopa and methyldopa) are developed. The first method involves the oxidation of o-dihydroxybenzene derivatives by N-bromosuccinimide followed by oxidative coupling with isoniazid leading to the formation of a red-coloured products of maximum absorbance (lambda(max)=480-490 nm). The second method is based on the formation of green to blue complex (lambda(max)=635-660 nm) between o- dihydroxybenzene derivatives and sodium nitroprusside in the presence of hydroxylamine hydrochloride. All measurements of the two procedures are carried out in an alkaline medium at room temperature. The two methods are successfully applied for the determination of dopamine hydrochloride, levodopa and methyldopa in injections and tablets of pharmaceutical preparation. The common excipients used as additives in pharmaceuticals do not interfere in the proposed methods. The reliability of these methods are established by parallel determination with the reported and official methods.     

Spectrophotometric methods for the determination of tolnaftate

Two simple and sensitive visible spectrophotometric methods (methods A and B) for the determination of tolnaftate in bulk samples and formulations are described. Method A (lambda(max) 490 nm) involves the reaction of tolnaftate with 2,6-dichloroquinone-4-chlorimide (DCQC: Gibb's reagent), while method B (lambda(max) 530 nm) is based on a similar reaction of the drug with p-N,N-dimethylphenylene diamine in the presence of chloramine-T. Both these methods are applicable to pure samples as well as formulations of the drug.     

Spectrophotometric methods for the determination of nifurtimox in bulk form and pharmaceutical formulations

Three simple and sensitive methods for the assay of Nifurtimox (NIF) which is an active antitrypanocide were developed. These methods are based on the formation of coloured species by treating either its reduction product with 3-methyl-2-benzothiazolinone hydrazone (MBTH) in the presence of ferric chloride (method A) or its hydrolysis product with 2-thiobarbituric acid (TBA) (method B) or by oxidizing it with excess N-bromosuccinamide (NBS) and determining the consumed NBS using p-N-methylaminophenol sulphate (metol)-isonicotinic acid hydrazide (INH) (method C). All variables have been optimized and the reaction mechanisms presented. Regression analysis of Beer's plot showed good correlation in the concentration range of 2.5-10, 2.5-30 and 1.25-7.5 microg/ml for methods A, B and C, respectively. No interference was observed from the additives and the validity of the methods was tested by analysing the tablets. Recoveries were 99.2-100.9%.     

Spectrophotometric determination of clozapine in pharmaceuticals

New Spectrophotometric methods for the assay of clozapine (CZP) in pure and dosage forms are described. Method A is based on the oxidative coupling reaction of CZP with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ceric ammonium sulphate to form a coloured species (_max 570 nm). Method B is also based on the oxidative coupling reaction of CZP withP-,N,N-dimethylpheny-lenediamine dihydrochloride (DMPD) in the presence of sodium hypochlorite to form a coloured species (_max 690 nm). Method C is based on the formation of coloured charge-transfer complex between CZP and chloranilic acid (_max 540 nm). Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 2–25, 10–120 and 15–300 g/ml for methods A, B and C, respectively. The validity of the proposed methods was tested by analysing pharmaceutical dosage forms containing CZP and the relative standard deviation values were within 1.0%.     

Four spectrophotometric methods for determination of nitrofurazone in pharmaceutical formulations

Four simple and sensitive visible spectrophotometric methods (A-D) for the determination of nitrofurazone in bulk samples and pharmaceutical formulations are described. They are based on the formation of colored species by treating either its reduction product with 3-methylbenzothiazolin-2-one hydrazone in the presence of ferric chloride (method A: _max 600 nm) or its hydrolysis product with thiobarbituric acid (method B: _max 520 nm, 440 nm) or barbituric acid (method C: _max 400 nm) or by oxidizing it with excess N-bromosuccinimide and determining the consumed NBS using metol-isonicotinic acid hydrazide (method D: _max 620 nm).     

Colorimetric determination of isoniazid and its pharmaceutical formulations

Two colorimetric methods for the estimation of isoniazid are developed. The first method depends on coupling of isoniazid with diazotized 1-amino anthraquinone zinc chloride salt (fast red AL salt) to form a red colour (lambda(max) 510 nm). The second one is based on the formation of a green complex (lambda(max) 655 nm) between the acid hydrazide and 2,6-dimethoxy-1,4-benzoquinone (DMBQ). All measurements of the two procedures were carried out in the presence of sodium hydroxide at room temperature (20 +/- 3 degrees C). The two methods are applied for the determination of isoniazid in presence of congenial drugs, vitamins and additives normally encountered with it in pharmaceutical dosage forms. The reliability of these methods was established by parallel determination with the reported and official methods.     

Spectrophotometric determination of azathioprine in pharmaceutical formulations

Four simple and sensitive visible spectrophotometric methods (A–D) have been described for the assay of azathioprine (ATP) either in pure form or in pharmaceutical formulations. Methods A and B are based on the oxidation of ATP with excess N-bromosuccinimide (NBS) or chloramine-T (CAT) and determining the consumed NBS or CAT with a decrease in colour intensity of celestine blue (CB) (method A) or gallocyanine (GC) (method B), respectively. Methods C and D are based on the diazotisation of reduced azathioprine (RATP) with excess nitrous acid and estimating either the consumed nitrous acid (HNO₂) with cresyl fast violet acetate (CFVA) (method C) or by coupling reaction of the diazonium salt formed with N-1-naphthyl ethylene diamine dihydrochloride (NED) (method D). All of the variables have been optimized and the reactions presented. The concentration measurements are reproducible within a relative standard deviation of 1.0%. Recoveries are 99.2–100.3%.     

Assay of cisapride in pharmaceutical formulations by extraction spectrophotometry

Four simple and sensitive spectrophotometric methods (A-D) for the assay of cisapride in pure and dosage forms based on the formation of chloroform soluble ion-associates under specified experimental conditions are described. Four acidic dyes, namely, Suprachen Violet 3B (SV 3B, method A), Erioglaucine A (EG-A, method B), Naphthalene Blue 12 BR (NB-12BR, method C) and Tropaeolin 000 (TP 000, method D) are utilized. The extracts of the ion-associates exhibit absorption maxima at 595, 640, 620 and 500 nm for methods A, B, C and D, respectively. Beer's law and the precision and accuracy of the methods are checked by the UV reference method. The results are reproducible with an accuracy of +/-1.0%. The methods are found to be suitable for the determination of cisapride in the presence of the other ingredients that are usually present in dosage forms.     

Organogermanium reactive intermediates. The direct detection and characterization of transient germylenes and digermenes in solution

Diphenylgermylene (Ph2Ge) and its Ge=Ge doubly bonded dimer, tetraphenyldigermene (6a), have been characterized directly in solution for the first time by laser flash photolysis methods. The germylene is formed via (formal) cheletropic photocycloreversion of 3,4-dimethyl-1,1-diphenylgermacyclopent-3-ene (4a), which is shown to proceed in high chemical (>95%) and quantum yield (phi = 0.62) by steady-state trapping experiments with methanol, acetic acid, isoprene, and triethylsilane. Flash photolysis of 4a in dry deoxygenated hexane at 23 degrees C leads to the prompt formation of a transient assigned to Ph2Ge (lambda(max) = 500 nm; epsilon(max) = 1650 M(-1) cm(-1)), which decays with second-order kinetics (tau approximately 3 micros), with the concomitant growth of a second transient species that is assigned to digermene 6a (tau approximately 40 micros; lambda(max) = 440 nm). Analogous results are obtained from 1,1-dimesityl- and 1,1-dimethyl-3,4-dimethylgermacyclopent-3-ene (4b and 4c, respectively), which afford Mes2Ge (tau approximately 20 micros; lambda(max) = 560 nm) and Me2Ge (tau approximately 2 micros; lambda(max) = 480 nm), respectively, as well as the corresponding digermenes, tetramesityl- (6b; lambda(max) = 410 nm) and tetramethyldigermene (6c; lambda(max) = 370 nm). The results for the mesityl compound are compared to the analogous ones from laser flash photolysis of the known Mes2Ge/6b precursor, hexamesitylcyclotrigermane. The spectra of the three germylenes and two of the digermenes are in excellent agreement with calculated spectra, derived from time-dependent DFT calculations. Absolute rate constants for dimerization of Ph2Ge and Mes2Ge and for their reaction with n-butylamine and acetic acid in hexane at 23 degrees C are also reported.     

Spectrophotometric and spectrofluorimetric methods for analysis of acyclovir and acebutolol hydrochloride

Simple and sensitive spectrophotometric and spectrofluorimetric methods are described for analysis of acebutolol hydrochloride. The proposed methods are based on oxidation of the selected drug with cerium(IV) ion in acidic medium with subsequent measurement of either the decrease in absorbance at 320 nm or the fluorescence intensity of the produced cerous(III) ion at 363 nm (excitation at 250 nm). Beer's law obeyed from 1.0-7.0 microg ml(-1) and 0.25-2.5 microg ml(-1) acebutolol hydrochloride, using the spectrophotometric and spectrofluorimetric method, respectively. The proposed methods were successfully applied for determination of the selected drug in its pharmaceutical preparation with good recoveries.     

Enzymatic inhibition enthalpimetry: The analytical potential of the inhibitory action of a series of physiologically active alkaloids on the activity of serum cholinesterase

A kinetic method is described for the enthalpimetric determination of a series of physiologically active alkaloids based on their inhibitory effect on the cholinesterase-catalysed hydrolysis of butyrylcholine iodide. All analyses are done at pH 8.0 and at 25.0°C (short term stability ± 0.002°C). Precision (< 3.0%) data are reported for the determination of physostigmine sulphate (1.0–4.0 × 10^-8), quinine sulphate (1.0 × 10^-6–4.0 × 10^-5), procaine hydrochloride (1.0 × 10^-5–× 2.5 × 10^-4), atropine sulphate (5.0 × 10^-5–3.0 × 10^-4), morphine sulphate (1.0–8.0 × 10^-4), codeine phosphate (3.0 × 10^-4–2.4 × 10^-3), pilocarpine nitrate (5.0 × 10^-4––6.0 × 10^-3) and thiamine hydrochloride (1.0–5.0 × 10^-3); the linear response ranges in mol dm^-3 are given in parentheses. Complete inhibition curves are presented and relative “potency” is inferred. The effects of several interfering inhibitors are discussed.