No full-text available
To read the full-text of this research,
you can request a copy directly from the authors.
Colorimetric Microdetermination of Bromhexine Drug in Aqueous Solution
Abstract
A simple, accurate and sensitive method for determination of bromhexine hydrochloride drug in aqueous
solution has been described. The procedure has been based on the reaction of this drug with an excess
amount of p-dimethylaminobenzaldehyde (DAB) in acidic medium (pH = 1.6) and the presence of sodium
dodecyl sulfate (SDS). The produced yellow color from this reaction has been followed spectrophotometrically
at an absorbance maximum of 430 nm. Microgram amounts of bromhexine hydrochloride can be
estimated with an accuracy of better than �1.5� and a relative standard deviation of less than 3.5�. The
method has been used for the determination of 0.41-82.5 �g.mL-1 with a molar extinction coefficient of
4699.1-3602.3 L.mol-1.cm-1.
An application of the developed procedure to bulk bromhexine hydrochloride and some of its pharmaceutical
preparations has been carried out. The effect of the presence of some other surfactants and common
pharmaceutical additives has been investigated. A comparison of the presented method with that in
the absence of SDS and the standard method of the British Pharmacopoeia has been explored. The suggestion,
according to the results, is to use the developed method as standard in pharmaceutical applications.
... It is well known that the aromatic amines are very easily oxidized by atmospheric oxygen, most are colorless when pure, and they are often encountered discolored by oxidation products [3]. However, the coloring 3 phenomenon that occurs in O-bromoaniline (from white to very dark or black color) deserves attention particularly by analytical chemists [4,5]. In actual, this compound is commercially delivered as a dark-colored solid in a sealed container which bears a label that reads "Keep under argon" (e.g. ...
... In order to prevent the freezing of such a compound (MP=32.0°C), the condenser should 4 be kept warm during distillation. However, a colorless liquid was obtained to give a pure white solid of O-bromoaniline [9]. ...
This short paper deals with the coloring phenomenon that occurs in O-bromoaniline from white to very dark. It is found that the very pure compound exhibits a significant resistance towards this phenomenon as stays for a long period without discoloring. Such a result is clearly of great interest to anyone who produces, marketing, or purchases and uses O-bromoaniline on a regular basis. The results show that the conventional methods for purification of solid compound such as recrystallization are not sufficient. It has been found that the fractional distillation under vacuum for this solid material gives a pure compound possesses a resistance against discoloring phenomenon. In particular, the listed purification procedure should allow chemical companies to produce and market a better quality product of O-bromoaniline.
... Figs. 13-16 explain the effect of SDS upon the forward and reverse rate constants, equilibrium constants, and infinite absorbance at different concentrations of DAB, respectively. The maxima of Fig. 13 are used for bimolecular reactions which attributed to the effect of concentration and dilution of reactants molecules by micelles [14]. In contrast, the relation for reverse rate constant in the presence of [SDS] exhibits a minimum (Fig. 14). ...
... It should be noted that some of the above results were employed for microdetermination of bromhexine in aqueous solution of SDS and applied successfully to its pharmaceutical preparations [14]. ...
Kinetic study of the condensation reaction of bromhexine with para-dimethylaminobenzaldehyde (DAB) in weakly acidic EthOH/H2O has
been investigated. An opposite first order reaction with respect to bromhexine and zero order with respect to DAB has been observed. The rate
constants, activation energies, frequency factors, and other related thermodynamic functions of activation for both forward and reverse reactions
have been determined. Standard thermodynamic parameters including equilibrium constant, �G◦, �H◦, and �S◦ have been calculated. The effect
of the presence of anionic surfactant (sodium dodecyl sulfate, SDS) upon these kinetic and thermodynamic parameters of this reaction in aqueous
solution has been examined. The results indicate that the presence of 4×10−3MSDS increase the forward and reverse rate constants together with
equilibrium constant by 104.3, 19.48, and 5.33 times, respectively. A substantial increase in the values of frequency factors of 1×105 and 2×104
for forward and reverse reactions, respectively, due to the presence of this amount of SDS has been detected. The observed positive sign of �S◦
in presence and absence of SDS has been confirmed through conductivity measurements. The rate constants in micellar phase, binding constants
between each bromhexine and DAB with SDS, and the change in standard chemical potential have been determined at different temperatures.
Activation energy, frequency factor, and other related thermodynamic functions of activation in micellar phase have also been calculated. It has
been concluded that the increases in the number of collisions between reactants molecules caused by presence of micelles plays a major role in the
physicochemical properties of surfactants solutions
... It is well known that the aromatic amines are very easily oxidized by atmospheric oxygen, most of the compounds are colorless when pure which they are often encountered discolored by oxidation products [4]. However, the coloring phenomenon that occurs in O-bromoaniline (from white to very dark or black color) deserves attention particularly by analytical chemists [5,6]. In actual, this compound is commercially delivered as a dark-colored solid in a sealed container, which bears a label that reads, "Keep under argon" (e.g. ...
This short paper deals with the coloring phenomenon that occurs in O-bromoaniline from white to very dark. It is found that the very pure compound exhibits a significant resistance towards this phenomenon as stays for a long period without discoloring. Such a result is clearly of great interest to anyone whom produces, marketing, or purchases and uses O-bromoaniline on a regular basis. The results show that the conventional methods for purification of solid compound such as recrystallization are not sufficient. It has been found that the fractional distillation under vacuum for this solid material gives a pure compound possesses a resistance against discoloring phenomenon. In other words, the conventional methods of purification cannot made absolute remove of impurities as the latter are responsible for the colouring phenomenon of the presented compound. In particular, the listed purification procedure should allow chemical companies to produce and market a better quality product of O-bromoaniline.
Simple, rapid, and sensitive ultraviolet-visible spectroscopy method was used to determine ultra-trace amounts of metformin (MET) in several samples such as drinking water, tablet, serum (blood), and urine without preconcentration step. Gold nanoparticles (AuNPs) were synthesized, and determination of MET was carried out based on the surface plasmon resonance property of AuNPs and the interaction between MET and AuNPs. Transmission electron microscopy (TEM) was utilized to characterize the structure of AuNPs before and after addition MET. Also, dynamic light scattering was used to investigate the size of nanoparticles distribution. The results showed that AuNPs were aggregated in the presence of the MET. Some parameters, including pH, AuNPs concentration, contact time, buffers, and ionic strength, were evaluated to select optimum conditions. Linear range obtained was 15–300 μg/L in the optimum conditions. Also, the correlation coefficient (R2), the limit of detection, and limit of quantification were equal to 0.9918, 0.99, and 1.12 μg/L, respectively. In addition, the effect of interfering species was investigated. Finally, the results of the analysis of different real samples indicated that the proposed method was suitable and accurate for determination of MET.
Poly(procaterol hydrochloride) (p-ProH) polymeric film was successfully deposited onto the carboxyl multi-walled carbon nanotube (CMWCNT) modified glass carbon electrode (GCE) to construct a p-ProH/CMWCNT composite modified GCE. Due to the synergistic effect of p-ProH and CMWCNT in the composite, the developed sensor can enormously enhance the oxidation peak current of bromhexine hydrochloride (BrH) at ca. + 0.90 V. Based on this appearance, an electrochemical method was established for the sensitive and selective determination of BrH with differential pulse voltammetry (DPV). Various conditions affecting the peak current response of BrH were studied and optimized. Under the best conditions, the oxidation peak current of BrH is linear to its concentration in two linear dynamic ranges of 0.2-1.0 μmol L ⁻¹ (R = 0.9948) and 1.0-8.0 μmol L ⁻¹ (R = 0.9956), with a detection limit of 0.1 μmol L ⁻¹ (S/N = 3). Interference experiment indicated that the as-prepared electrochemical sensor showed wonderful selectivity to the recognition of BrH and was free from disturbance of many other electro-active substances such as dopamine, ascorbic and uric acid. Finally, the practicability of the BrH sensor was verified by the satisfactory results acquired from the BrH determination in pharmaceutical preparation and human serum.
In this paper, the electrochemiluminescence (ECL) behavior of luminol/H2O2 system in the presence of bromhexine hydrochloride (BrH) was investigated. It was found that the ECL intensity of luminol/H2O2 system on a platinum electrode could be intensely quenched by BrH owing to the scavenging superoxide radical ability of BrH, and therefore the sensitive determination of BrH was possible. Under optimal conditions, the quenched ECL intensity was linear to the concentration of BrH in a wide range of 0.08 to 500 μM, with a detection limit of 0.02 μM (signal‐to‐noise ratio (S/N) = 3). This ECL method possessed the merits of rapid, simple and sensitive, and was successfully applied to the BrH quantification in pharmaceutical preparations with satisfactory recoveries of 91.0 ± 4.0 to 106.5 ± 3.4%. The possible route of the quenched ECL of luminol/H2O2 in the presence of BrH was also discussed.
In pH 4.2–5.2 HOAc-NaOAc buffer solution, Ag+ reacted with dihalogenated fluorescein (DHF) dyes to form a 1:2 anionic complex. This anionic complex could further react with hyoscine butylbromide (HBB) to form 1:1 ion-association complex, which resulted in the significant enhancement of resonance Rayleigh scattering (RRS) intensity. Therefore, a novel method for the determination of HBB by resonance Rayleigh scattering (RRS) coupled with flow injection analysis (FIA) technique has been established. The present method had been applied to determine HBB in capsules and the results were in good agreement with those obtained by the literature method.
The present paper firstly announces the possibility of using a Schiff base as an acid-base indicator. This surprising phenomenon can be considered as an interest due to the fact that Schiff bases are usually unstable in solutions and definitely undergo hydrolysis. It was found that such a specific observation depends merely upon the chemical structure and type of the substitute of amine that reacts with aldehyde to give the Schiff base. The latter reagent 4((4-dimethylamino-benzylidene)-amino)- benzene sulfonamide was synthesized from the condensation of sulfanilamide with p-dimethylaminobenzaldehyde. The reagent solution shows a reproducible change in its color due to the addition of acid and base. A UV-Vis spectroscopic characterization and acid-base equilibrium study of the reagent for its possible use as an indicator were investigated. The results show that the reagent is an amphoteric which possesses four ionization constants Ka1, Ka2, Kb1 and Kb2 of weak dibasic and diacidic properties. The value of pKa2 (9.80) is parallel to the observed transition interval pH 9.5 (yellow) and pH 10.5 (colorless), which is considered to be the indicator exponents pKi. It was concluded that the benzyl sulfonamide group plays a key role in the stability of the reagent towards hydrolysis and also for indicator characteristics through breaking the conjugation.
Benzocaine is well known as an insoluble substrate in water. Therefore, its physical and analytical treatments in
the presence of surfactant may allow organic solvents to be replaced by aqueous surfactants solutions. The effect of
the presence of anionic surfactant (sodium dodecyl sulfate, SDS) upon the condensation reaction of benzocaine with
water insoluble p-dimethylaminobenzaldehyde (DAB) in aqueous solution has been investigated extensively. The
presence of 5x10-3M SDS increases the reaction rate by 20 times in contrast to that of a solution in 20% ethanol. A
substantial increase in absorption band due to the formed Schiff base followed by a red shift has been observed. A
great advantage in analytical application resulting from the presence of surfactant due to the formation of a charge
transfer complex has been reported. The latter phenomenon has been realized and proved in this study, which
depends merely on the charge of micelle surface. A simple, accurate, and sensitive method for microdetermination of
benzocaine in aqueous surfactant solution has been introduced. The proposed procedure for analysis of the presented
drug in its bulk form and pharmaceutical formulations is more sensitive and accurate than that of the British
pharmacopoeia method. It has been concluded that the replacing of organic co-solvents by surfactants was not only
captured for avoiding their pollution and toxic implication but there are some advantages gained from the presence
of surfactant molecules. The used surfactant compound (SDS) in this study is quite green and is commonly used as a
detergent in toothpaste.
A gradient high-performance liquid chromatographic method for the simultaneous determination of an anti-cold drug was reported. Nine components in the preparation, such as acetaminophen, anhydrous caffeine, riboflavin, dihydrocodeine phosphate, DL-methylephedrine hydrochloride, carbinoxamine maleate, noscapine, bisibuthiamine and bromhexine hydrochloride, could be completely separated by changing from water-acetonitrile (95: 5) to water-acetonitrile (1: 1) as the mobile phase containing 0.1% of phosphoric acid and 0.08w/v% of sodium heptansulfonate by a linear gradient program. The time required for the analysis was about 40 minutes, and the time for initializing was about 15 minutes. Under this method, the recoveries of these components were 99.9~ 100.4%, and showed good reproducibility for each component. The results of the determination were in good agreement with the conventional method. © 1997, The Japan Society for Analytical Chemistry. All rights reserved.
Ullmann's Encyclopedia of Industrial Chemistry is the fifth completely revised edition of Ullmann's Encyklopaedie der Technischen Chemie, the fourth edition of which was completed in 1984. The fifth edition began with volume Al in 1985 and is expected to be completed in thirty-six volumes by 1996, three or four volumes appearing each year. A cumulative index will be published each year to provide access to published volumes. This reviewer had volumes A1 through A7 (1985–1986) and the Index to Volumes A1 to A4 (Abrasives to Calcium Sulfate) (1986) available for review. The most noticeable difference between the fourth and fifth editions is “publication of the Encyclopedia in the English language rather than in the German of its predecessors.” (editors' preface to vol. A1) Thus, it can now join the ranks of the other prominent encyclopedia of chemical technology and industry: Kirk-Othmer Encyclopedia of Chemical Technology (Wiley-Interscience, 3d ed., 1978–84, 25 vols.). Another comprehensive chemical engineering encyclopedia, Encyclopedia of Chemical Processing and Design (John J. McKetta, editor; Dekker, 1976) is incomplete, as of this writing, volume 27 (covering through lectone dimethyl) being the latest to have been published. Since the first edition is incomplete and not as well established in the chemical technology community, the Encyclopedia of Chemical Processing and Design will not be discussed here. Anyone interested in a comparative review of all three encyclopedias is referred to the review by Jay Matley entitled “Ullmann's Encyclopedia of Industrial Chemistry,” which appeared in Chemical Engineering (vol. 93, no. 8 [28 April 1986]: 95–98). This review will compare the fifth edition of Ullmann's Encyclopedia of Industrial Chemistry with the third edition of Kirk-Othmer Encyclopedia of Chemical Technology (the two works will be referred to as Ullmann and Kirk-Othmer, respectively).
Kinetic study of the condensation reaction of bromhexine with para-dimethylaminobenzaldehyde (DAB) in weakly acidic EthOH/H2O has
been investigated. An opposite first order reaction with respect to bromhexine and zero order with respect to DAB has been observed. The rate
constants, activation energies, frequency factors, and other related thermodynamic functions of activation for both forward and reverse reactions
have been determined. Standard thermodynamic parameters including equilibrium constant, �G◦, �H◦, and �S◦ have been calculated. The effect
of the presence of anionic surfactant (sodium dodecyl sulfate, SDS) upon these kinetic and thermodynamic parameters of this reaction in aqueous
solution has been examined. The results indicate that the presence of 4×10−3MSDS increase the forward and reverse rate constants together with
equilibrium constant by 104.3, 19.48, and 5.33 times, respectively. A substantial increase in the values of frequency factors of 1×105 and 2×104
for forward and reverse reactions, respectively, due to the presence of this amount of SDS has been detected. The observed positive sign of �S◦
in presence and absence of SDS has been confirmed through conductivity measurements. The rate constants in micellar phase, binding constants
between each bromhexine and DAB with SDS, and the change in standard chemical potential have been determined at different temperatures.
Activation energy, frequency factor, and other related thermodynamic functions of activation in micellar phase have also been calculated. It has
been concluded that the increases in the number of collisions between reactants molecules caused by presence of micelles plays a major role in the
physicochemical properties of surfactants solutions
A novel flow-based procedure involving the multi-pumping approach was developed for the spectrophotometric determination of bromhexine in pharmaceutical preparations. The method is based on reaction with 3-methyl-2-benzothiazolinone hydrazone (MBTH) and Ce(IV). Several solenoid micro-pumps are present in the manifold in order to provide improved system control. Critical tasks in continuous flow analysis, sample–reagent introduction and solution propelling, are then efficiently carried out. Moreover, the pulsed flow inherent to the mini-pumps ensures good mixing conditions, thus improving the reaction zone homogenisation. This aspect becomes particularly attractive for the implementation of analytical procedures involving several consecutive reactions as it happens with the proposed procedure.Linear calibration plots (r>0.995, n=6) were obtained for bromhexine concentrations up to 400 mg l−1. Detection limit was 2 mg l−1 and the sampling rate was about 45 samples h−1. Results are precise (R.S.D.<1.5%; n=10) and in agreement with those furnished by the reference procedure involving a potentiometric titration.
Kinetics of condensation reactions of six sulpha drugs (I-VI) with p-dimethylaminobenzaldehyde (DAB) in a weakly acidic EthOH/H2O solution have been studied spectrophotometrically. The reaction was found to be first order with respect to DAB and zero order with respect to sulphonamide. The rate constants, activation energies, and other related thermodynamic functions have been determined. The effect of the presence of anionic surfactant sodium dodecyl sulphate (SDS) on the kinetics of this reaction in aqueous solution has been investigated. The observed rate constants increase with increasing the amount of SDS except for those of sodium sulphacetamide (VI). The surfactant molecules enhance the reaction rates (14-113 times) in concentrations less than critical micellar concentration (cmc). A developed spectrophotometric method for determining sulphonamides in aqueous solution by their reactions with an excess of DAB in the presence of SDS and HCl (pH = 2) at a wavelength of 447 nm has been introduced. Microgram amounts of sulphonamides can be estimated with accuracy better than ± 1.5% and reproducibility less than ± 0.064%. The results of application to sulphonamides in pure form indicate that the presented method is simple, sensitive, precise, accurate, and comparable to the colorimetric Bratton-Marshall standard procedure. The effect of interferences and application of the presented method to two pharmaceutical preparations have been investigated.
Yields of colored Schiff base products of the reversible condensation of 6-aminopenicillanic and 7-aminocephalosporanic acids with para-dimethylaminobenzaldehyde in a weakly acid aqueous solution strongly increase in the presence of micelles of sodium dodecyl sulfate. The binding constants of reactants and products of both reactions to micelles were calculated from the concentration profiles of micellar effects on rates and equilibrium of the condensation reactions. The observed micellar-induced shifts of equilibrium are accompanied by strong acceleration of the forward and small retardation of backward processes. Some deviations from the theoretical profiles due to saturation of micelles with reactants were observed. The colored form of the reaction product was found to be the protonated Schiff base. Its stability in time is strongly enhanced in the micellar medium. The spectrophotometric determination of title compounds under optimum micellar conditions possesses ca. 300 times higher sensitivity than the standard procedure.
- M D Shingbal
- V R Rao
Shingbal, M. D.; Rao, V. R. Indian Drugs 1985, 22, 275;
Chem. Abst. 1985, 103, 92947k.
- R A Khalil
- B Khiro
Khalil, R. A.; Al-Khiro, B. Z. J. Chin. Chem. Soc. 2006, 53,
637.
Liquids; accepted for publication 25
- R A Khalil
- R Khayat
Khalil, R. A.; Al-Khayat, R. Z. Phys. Chem. Liquids; accepted for publication 25 Oct. 2006.
- R Canals
- J M Caldero
- Afinidad
Canals, R.; Caldero, J. M. Afinidad 1980, 37, 435; Chem.
Abst. 1981, 94, 145452z.
- M Masuda
- T Satoh
- M Handa
- Y Itoh
Masuda, M.; Satoh, T.; Handa, M.; Itoh, Y.; Sagara, K.
Bunseki Kagaku 1997, 46, 777.
- E Bechgaard
- A J Neilsen
- Chromatogr
Bechgaard, E.; Neilsen, A. J. Chromatogr. 1982, 228, 392;
Chem. Abst. 1982, 96, 154935c.
Microdetermination of
- A M A M S Saeed
- Thesis
Saeed, A. M. A. M. S. Thesis, Mosul University, Nov. 2005.
Microdetermination of Bromhexine Drug
J. Chin. Chem. Soc., Vol. 54, No. 4, 2007 1105
- M L Chainani
- A M Nighojkar
- S D Naik
Chainani, M. L.; Nighojkar, A. M.; Naik, S. D. Indian Drugs
1986, 24, 51; Chem. Abst. 1987, 106, 107977h.
- G R Rao
- S Raghuveer
- P Khadgapathi
Rao, G. R.; Raghuveer, S.; Khadgapathi, P. Indian Drugs
1987, 25, 125; Chem. Abst. 1988, 109, 27663z.