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Biomedical subjects

M M Ghoneim

Publications and source records attributed to M M Ghoneim.

At least 19 recordsLinked to original sources

Voltammetry and quantification of the contraceptive drug norethisterone in bulk form and pharmaceutical formulation.

The electrochemical behavior of norethisterone at the mercury electrode was studied in the universal buffer of various pH values using dc-polarography, cyclic voltammetry and controlled-potential electrolysis. Norethisterone was reduced at the mercury electrode via the consumption of two electrons corresponding to reduction of the 3-keto-delta-4-group in the A-ring of the molecule. The pK(a) value (8.7) of norethisterone was determined from the polarographic and spectrophotometric measurements. A fully validated, simple, sensitive, precise and inexpensive square-wave adsorptive cathodic stripping (SWAdCS) voltammetry procedure was described for trace quantification of bulk norethisterone. The stripping voltammetry peak current of norethisterone in a universal buffer of pH 5 following its accumulation onto the hanging mercury drop electrode (HMDE) at -0.6 V (versus Ag/AgCl/KCl(s)) for 130 s showed a linear response with the concentration over the range 5 x 10(-9) to 3 x 10(-7)M norethisterone. Detection and quantitation limits of 1.5 x 10(-9) and 5 x 10(-9)M bulk norethisterone, respectively, were achieved. The proposed procedure was successfully applied for the assay of norethisterone in Steronate tablets without interference from excipients.

Buffers↗

Voltammetric assay of the anthelmintic veterinary drug nitroxynil in bulk form and formulation at a mercury electrode.

The electrochemical behavior of the anthelmintic veterinary drug nitroxynil at the mercury electrode was studied in a series of Britton-Robinson universal buffer of pH 1.9-11 containing 20% (v/v) ethanol using dc-polarography cyclic voltammetry and controlled-potential coulometry. The voltammograms exhibited two irreversible cathodic steps over the pH range 1.9-10.2; the height of the first step is double that of the second one. Controlled-potential coulometry in the B-R universal buffer of pH 1.9-10 at a mercury pool working electrode revealed the consumption of four and two electrons via the first and second reduction steps, respectively, which attributed to reduction of the NO2 group to the hydroxylamine stage (first step), and then to the amine stage (second step). Three voltammetric analytical procedures including dc-polarography, differential-pulse adsorptive stripping voltammetry and square-wave adsorptive stripping voltammetry were optimized for the direct determination of bulk nitroxynil. The three proposed procedures were applied for analysis of bulk nitroxynil with limits of detection of 3 x 10(-5), 1.31 x 10(-8) and 8.4 x 10(-10)M and limits of quantification of 1 x 10(-5), 4.36 x 10(-8) and 2.80 x 10(-9)M, respectively. The three procedures were successfully applied to the determination of nitroxynil in formulation (Dovenix, 25% nitroxynil injection solution) without the necessity for sample pretreatment and/or time-consuming extraction steps prior to the analysis.

Antiplatyhelmintic Agents↗

Adsorptive cathodic stripping voltammetric assay of the estrogen drug ethinylestradiol in pharmaceutical formulation and human plasma at a mercury electrode.

The electroreduction of ethinylestradiol at the hanging mercury drop electrode in the Britton-Robinson universal buffer of pH 2-11 was studied and its interfacial adsorptive character onto the mercury electrode surface was identified. A validated simple, rapid, sensitive, specific, precise and inexpensive square-wave voltammetric procedure is described for the determination of ethinylestradiol following its accumulation onto a hanging mercury drop electrode in a Britton-Robinson universal buffer of pH 7. The optimal procedural conditions were: accumulation potential E(acc)=-0.7 V versus Ag/AgCl/KCl(s), accumulation duration=60s, pulse-amplitude=70 mV, scan increment=10 mV and frequency=120 Hz. Limits of detection (LOD) and quantification (LOQ) of 5.9x10(-10)M and 1.9x10(-9)M bulk ethinylestradiol, respectively, were achieved. The proposed procedure was successfully applied to the quantification of ethinylestradiol in pharmaceutical formulation (Ethinyl-oestradiol tablets) and in human serum and plasma without the necessity for sample pretreatments and/or time-consuming extraction or evaporation steps prior to the analysis. LOD of 8.7x10(-10)M and 3x10(-9)M and LOQ of 2.9x10(-9)M and 1x10(-8)M of ethinylestradiol were achieved in human serum and plasma, respectively.

Adult↗

Voltammetric behavior and assay of the antibiotic drug cefazolin sodium in bulk form and pharmaceutical formulation at a mercury electrode.

The electrochemical behavior of the antibiotic drug cefazolin sodium (CFZ) in Britton-Robinson buffers (pH 2-11) at the mercury electrode was studied by means of dc-polarography, cyclic voltammetry, controlled-potential coulometry and square-wave adsorptive stripping voltammetry techniques. A validated square-wave adsorptive cathodic stripping voltammetric procedure was described for the trace determination of cefazolin in bulk form up to limits of detection and quantitation of 2.6 x 10(-10)M and 8.6 x 10(-10)M, respectively. The method was successfully applied for determination of cefazolin in pharmaceutical preparation without the necessity for samples pretreatment or any time-consuming extraction or evaporation steps prior to the analysis.

Anti-Bacterial Agents↗

Assay of the anti-psychotic drug haloperidol in bulk form, pharmaceutical formulation and biological fluids using square-wave adsorptive stripping voltammetry at a mercury electrode.

The cyclic voltammetric behavior of haloperidol at a hanging mercury drop electrode was studied in Britton-Robinson buffer series of pH 2.5-11 containing 40% (v/v) ethanol. A single two-electron irreversible cathodic peak was obtained which attributed to reduction of the CO double bond. In addition, a small enhanced adsorptive pre-wave was observed at less negative potentials over the pH range 3.5-11. Controlled adsorptive accumulation of haloperidol onto the hanging mercury drop electrode provided the basis for its direct trace assay in bulk form, pharmaceutical formulation and human biological fluids using square-wave adsorptive cathodic stripping voltammetry. Following preconcentration of bulk haloperidol onto the HMDE a well-developed square-wave cathodic peak was generated in Britton-Robinson buffer especially at pH values 9-10; its peak current showed a linear dependence on the concentration of haloperidol over the range 1 x 10(-9)M to 1.5 x 10(-6)M depending on the preconcentration duration. The procedural parameters for assay of haloperidol were studied. The achieved limits of detection (LOD) and quantitation (LOQ) were 3.83 x 10(-10)M and 1.28 x 10(-9)M bulk haloperidol, respectively. The procedure was successfully applied to assay haloperidol in tablets (Safinace) and in spiked human serum and urine. LOD of 3.3 x 10(-9)M and 5.46 x 10(-9)M, and LOQ of 1.10 x 10(-8) and 1.82 x 10(-8)M haloperidol were achieved in spiked human serum and urine samples, respectively.

Electrochemistry↗

Adsorptive stripping voltammetric quantification of the antipsychotic drug clozapine in bulk form, pharmaceutical formulation and human serum at a mercury electrode.

Using the cyclic voltammetry technique and the Britton-Robinson buffer (pH 2-10) as a supporting electrolyte, clozapine was found to reduce at the hanging mercury drop electrode in a single two-electron irreversible step corresponding to reduction of the azomethine group of the seven-member heterocyclic ring. Based on the interfacial adsorptive character of clozapine onto the hanging mercury drop electrode, a validated square-wave adsorptive cathodic stripping (SWAdCS) voltammetric procedure was described for the quantification of bulk clozapine with limits of detection and quantitation of 4.5 x 10(-10) and 1.5 x 10(-9) M, respectively. The proposed procedure was successfully applied to the quantification of the drug in pharmaceutical formulation (Leponex) and human serum without the necessity for samples' pretreatment or any time-consuming extraction or evaporation steps prior to the analysis. The limits of detection and quantitation of clozapine in spiked human serum were found to be 1 x 10(-9) and 3.3 x 10(-9) M, respectively. The proposed procedure for quantification of clozapine in bulk form, tablets and human serum has the advantage of being simple, rapid, sensitive, precise and inexpensive compared to most of the reported methods.

Antipsychotic Agents↗

Electrochemical behavior and determination of amiloride drug in bulk form and pharmaceutical formulation at mercury electrodes.

The polarographic behavior of amiloride hydrochloride has been studied in Britton-Robinson buffers of pH 1.9-11. In acidic medium at Ph< or =2, the dc-polarograms exhibited a single 4-electron cathodic irreversible wave, while at pH values >2, a second two-electron irreversible cathodic wave appeared at a more negative potential. The single or first wave may be attributed to the cleavage of the double bond of the -CH=NH of the imidino amide group with the release of NH(3). While the second wave may be due to the saturation of the C=O of the carboxamide moiety. A polarographic procedure of suffocate sensitivity for the determination of bulk amiloride drug in Britton-Robinson buffer at pH 2 is described. The calibration graph was obtained over the concentration range 2.5 x 10(-5) to 2.5 x 10(-4) M amiloride. The limits of detection (LOD) and quantitation (LOQ) of the procedure were 1 x 10(-5) and 3.3 x 10(-4) M bulk amiloride, respectively. Moreover, a differential-pulse adsorptive cathodic stripping voltammetric procedure has been described to assay of the drug at lower concentration levels. The optimal conditions were: E(acc) = -0.9V, t(acc)=30 s, scan rate=20mV, pulse-height=90 mV and Britton-Robinson buffer of pH 8. The calibration graph was obtained over the concentration range 2 x 10(-8) to 1 x 10(-6) M for bulk amiloride. Both procedures were successfully applied to the determination of amiloride in tablets without the necessity for sample pretreatment or any time-consuming extraction or evaporation steps prior to the drug analysis.

Amiloride↗

Voltammetric behavior and quantification of the sedative-hypnotic drug chlordiazepoxide in bulk form, pharmaceutical formulation and human serum at a mercury electrode.

Chlordiazepoxide is a sedative-hypnotic drug widely employed as a transquilizer and anti-depressant. Its electrochemical behavior in Britton-Robinson (B-R) buffers of pH 2-11 at a mercury electrode has been investigated using dc-polarography, cyclic voltammetry and controlled-potential coulometry. Polarograms of the drug in B-R buffers of pH 2-10 exhibited three 2-electron waves, while at pH>10, only a single 4-electron wave was observed. The first, second, and third waves in buffers of pH 10) may be due to the reduction of both the N-oxide and C=N centers in a one step. The shift of the E(1/2,) values to more negative potentials upon the increase of pH indicated the involvement of protons in the electrode reaction and that the proton-transfer reaction precedes the electrode process proper. The estimated data indicated that, one proton and two electrons are participated in the rate-determining step of each of the reduced centers. The general sequence of chlordiazepoxide reduction processes via each of its reactant centers may be expressed as: H(+), e, e, H(+)((fast)).Based on the interfacial adsorptive character of the drug onto the mercury electrode, a validated direct square-wave adsorptive cathodic stripping (SWAdCS) voltammetric procedure has been described for the trace determination of the drug in bulk form, tablets and human serum. The procedure did not require sample pretreatment or time-consuming extraction or evaporation steps prior to the assay of the drug. The optimized operational conditions of the proposed procedure have been found to be: accumulation potential E(acc.)=-0.9 V, accumulation time t(acc.)=30s, pulse-amplitude=50 mV, scan increment=10 mV and frequency=120 Hz. The proposed procedure is much more simple, fast, sensitive, costly low and achieved much more lower limits of detection (LOD) (4.4 x 10(-10)M and 6.6 x 10(-10)M) and limits of quantitation (LOQ) (1.5 x 10(-9)M and 2.2 x 10(-9)M), respectively in pharmaceutical formulation and spiked human serum, compared to previously reported methods.

Chemistry, Pharmaceutical↗

Electrochemical behavior of the antituberculosis drug isoniazid and its square-wave adsorptive stripping voltammetric estimation in bulk form, tablets and biological fluids at a mercury electrode.

Isoniazid, pyridine-4-carboxylic acid hydrazide, is an antituberculosis-agent, which is used to prevent the development of clinical tuberculosis. A validated square-wave adsorptive cathodic stripping voltammetric procedure for the trace determination of the bulk drug at the hanging mercury drop electrode (HMDE) has been developed. Under the optimized conditions, (accumulation potential=-0.9 V, accumulation time=50-300 s, scan increment=8 mV, pulse-amplitude=25 mV, frequency=120 Hz and acetate buffer at pH 5.5) isoniazed generated two irreversible cathodic peaks. The first peak current showed a linear dependence with the drug concentration over the range 5 x 10(-10)-21 x 0(-6) M. The mean percentage recoveries, based on the average of five replicate measurements, for 7 x 10(-9) and 5 x 10(-8) M isoniazid were 97.71+/-2.93 and 99.76+/-0.77, respectively. The achieved limits of detection (LOD) and quantitation (LOQ) were 1.18 x 10(-10) and 3.93 x 10(-10) M isoniazid, respectively. The procedure was applied to the assay of the drug in tablets (Isocid and T.B. Zide), spiked human serum and urine with mean percentage recoveries of 97.81+/-1.49, 97.45+/-2.09, and 97.08+/-1.06, respectively. The limits of detection of 1.47 x 10(-9) and 2.4 x 10(-8) M, and quantitation of 4.9 x 10(-9) and 8 x 10(-8) M drug in human serum and urine, respectively, were achieved. The mean values of the various pharmackinetic parameters of isoniazid (C(max), T(max), t(1/2), AUC, and K(e)), estimated from analysis of plasma of two volunteers by means of the proposed procedure were similar to literature values.

Adult↗

Square-wave adsorptive cathodic stripping voltammetric determination of anti-inflammatory indomethacin drug in tablets and human serum at a mercury electrode.

Indomethacin is a non-steroidal anti-inflammatory drug possessing anti-pyretic and analgesic properties. A fully validated square-wave adsorptive cathodic stripping voltammetric procedure is described for determination of indomethacin. The procedure was based on the reduction of the C=O double bond of the drug molecule in Britton-Robinson buffer (pH 4) after its preconcentration onto the mercury electrode surface. The optimized conditions of the procedure were: frequency 120 Hz, scan increment 10 mV, pulse amplitude 50 mV, preconcentration potential -0.9 V (vs. Ag/AgCl/KCl(s)) and preconcentration time 90 s. The proposed procedure was successfully applied for determination of the drug in tablets and human serum with good recoveries. The limits of detection in bulk form and human serum were 6.7 x 10(-10) mol L(-1) and 8.1 x 10(-10) mol L(-1), respectively.

Adsorption↗

Cathodic adsorptive stripping square-wave voltammetric determination of nifedipine drug in bulk, pharmaceutical formulation and human serum.

Nifedipine is a calcium-channel antagonist drug used in the management of angina pectoris and hypertension through inhibition of calcium influx. A fully validated sensitive cathodic adsorptive stripping square-wave voltammetry procedure was optimized for the determination of the drug at trace levels. The procedure was based on the reduction of the nitrophenyl group after the interfacial accumulation of the drug onto a hanging mercury drop electrode in Britton-Robinson buffer of pH 11.0. The optimal conditions of the procedure were found to be: accumulation potential=-0.9 V vs. Ag/AgCl/KCl(s)), accumulation time=30 s, scan increment=10 mV, pulse amplitude=50 mV and frequency=120 Hz. Under these conditions, a well-defined peak was obtained; its peak current showed a linear dependence on drug concentration in the range of 2x10(-9)-2x10(-7) mol L(-1) bulk nifedipine. The mean recoveries based on eight replicate measurements for 1x10(-8) and 5x10(-8) mol L(-1) bulk nifedipine solutions were 98.46+/-0.86% and 98.23+/-0.92%, respectively. A detection limit of 3.42x10(-10) mol L(-1) bulk nifedipine was achieved. The procedure was successfully applied for assay of the drug in tablets and spiked human serum with mean recoveries of 101.95+/-1.42% and 98.70+/-0.63%, respectively. The limit of detection of the drug in spiked human serum was found to be 3.90x10(-10) mol L(-1).

Calcium Channel Blockers↗

Direct determination of praziquantel in pharmaceutical formulations and human plasma by cathodic adsorptive stripping differential-pulse voltammetry.

The polarographic and cyclic voltammetric behaviour of praziquantel was studied in B.R. buffers of different pH values. Contradictory to that mentioned in a previously published work, praziquantel is an electro-active compound. Its polarogram exhibited a single 2-electron irreversible reduction wave in B.R. buffer of pH 5, the wave height decreased on the increase of pH till it disappeared in solution of pH >7. This wave was attributed to the reduction of the Cz.dbnd6;O double bond. The quantitative trace determination of bulk praziquantel was studied at a hanging mercury drop electrode by cathodic adsorptive stripping differential-pulse voltammetry. A fully validated sensitive procedure based on controlled adsorptive accumulation of the drug onto a HMDE was developed for its direct determination without derivatization. Accumulation of praziquantel was found to be optimized in 0.1 M Na(2)SO(4) solution as supporting electrolyte under the following conditions: accumulation potential, -1.2 V (vs. Ag/AgCl/KCl(s)); accumulation time, 30 s; scan rate, 10 mV/s and pulse height 100 mV. The proposed procedure was applied successfully for determination of praziquantel in its pharmaceutical formulations and human plasma. The mean recoveries of the drug were 98.85-99.42% and 99.12-100.47% with RSD of 0.49-0.95% and 0.45-0.52% in pharmaceutical formulations and human plasma, respectively. Limits of detection and quantitation of 1.14x10(-9) and 3.80x10(-9) M praziquantel, respectively, were achieved.

Adsorption↗

Assay of dipyridamole in human serum using cathodic adsorptive square-wave stripping voltammetry.

A rapid and sensitive square-wave voltammetric procedure was optimized for the determination of dipyridamole after its adsorption preconcentration onto a hanging mercury drop electrode. The peak current of the first of the two peaks developed for this drug in Britton-Robinson buffer at pH 8.0 has been considered for the present analytical study. An accumulation potential of -1.0 V versus Ag/AgCl/KCl(s), pulse amplitude a =100 mV, scan increment Delta E =10 mV, and frequency f =120 Hz were the optimal experimental parameters. Dipyridamole can be determined in the concentration range of 9.0 x 10(-9) to 5.0 x 10(-6) M using accumulation times of 30-300 s. A detection limit of 4.0 x 10(-11) M was achieved after a 300 s accumulation time. Applicability to serum samples was illustrated. The average recoveries for dipyridamole spiked to serum at 0.25-4.50 micro g ml(-1) were 96.0-102.0%, and the higher standard deviation was 2.9%. A detection limit of 0.06 micro g mL(-1) of serum was obtained.

Dipyridamole↗

Electrochemical reduction of meloxicam at mercury electrode and its determination in tablets.

The electrochemical reduction of meloxicam has been studied at a mercury electrode using various electrochemical methods in aqueous solutions over a wide pH range. The reduction of the drug produced a single reduction step in acidic media, whereas in slightly acidic and neutral media two reduction steps were observed. In alkaline media meloxicam shows a single pH-independent reduction step. The irreversibility of the electrode process was verified by different criteria. At all pH values, reactant adsorption at mercury electrode was observed. The mechanism of reduction was discussed. Using differential-pulse voltammetry, the drug yielded a well-defined voltammetric response in Britton-Robinson buffer solution, pH 4.0 at -1.286 V (vs. Ag/AgCl). This process could be used to determine meloxicam concentration in the range 1.0 x 10(-8)-5.0 x 10(-6) M. The method was successfully applied for the analysis of meloxicam in the tablet dosage form.

Anti-Inflammatory Agents, Non-Steroidal↗

Determination of trimetazidine HCl by adsorptive stripping square-wave voltammetry at a glassy carbon electrode.

The adsorptive and electrochemical behavior of trimetazidine hydrochloride on a glassy carbon electrode were investigated in acetate buffer solution by using cyclic and square-wave voltammetry. Cyclic voltammetric studies indicated the oxidation of trimetazidine hydrochloride at the electrode surface through a single two-electron irreversible step and fundamentally controlled by adsorption. The solution condition and instrumental parameters were optimized for the determination of the authentic drug using adsorptive square wave stripping voltammetry. Trimetazidine hydrochloride gave a sensitive adsorptive oxidative peak at 0.750 V (vs. Ag/AgCl). The oxidation peak was used to determine authentic trimetazidine hydrochloride concentration in the range 5.0 x 10(-8)-5.0 x 10(-6) M with a detection limit of 2.0 x 10(-8) M. The procedure was successfully applied for assay of trimetazidine hydrochloride in the tablet dosage form (Vastarel). A mean recovery of 94.7% with a relative standard deviation (R.S.D.) of 0.88% was obtained. Applicability to assay the drug in urine samples was illustrated. The peak current was linear with the drug concentration in the range 17-85 microg per ml urine. The detection limit was 1.7 microg ml(-1) urine.

Drug Stability↗

Effects of frequent marijuana use on memory-related regional cerebral blood flow.

It is uncertain whether frequent marijuana use adversely affects human brain function. Using positron emission tomography (PET), memory-related regional cerebral blood flow was compared in frequent marijuana users and nonusing control subjects after 26+ h of monitored abstention. Memory-related blood flow in marijuana users, relative to control subjects, showed decreases in prefrontal cortex, increases in memory-relevant regions of cerebellum, and altered lateralization in hippocampus. Marijuana users differed most in brain activity related to episodic memory encoding. In learning a word list to criterion over multiple trials, marijuana users, relative to control subjects, required means of 2.7 more presentations during initial learning and 3.1 more presentations during subsequent relearning. In single-trial recall, marijuana users appeared to rely more on short-term memory, recalling 23% more than control subjects from the end of a list, but 19% less from the middle. These findings indicate altered memory-related brain function in marijuana users.

Analysis of Variance↗

Chronic drug use and cognitive impairments.

Reports regarding the effects of chronic drug use on human cognition and comparisons of different drug user groups have been inconsistent. Methodological flaws may account for some inconsistencies. To determine the effects of chronic drug use on cognition, drug users (n=192) were tested 17.1+/-0.3 days (mean+/-S.E.) and 99.4+/-1.7 days on average after their last use of drugs before beginning treatment. Drug users were categorized as stimulant, alcohol, or polydrug users. Their performance on tests of academic achievement, verbal memory, and abstraction was compared to performance of community-dwelling controls (n=137). The groups were matched on selected demographic and psychiatric characteristics. Historical records of achievement test scores were used to attempt to control for premorbid intellectual ability. Drug users showed impairments on each of the achievement tests (P<.001), as well as poorer total recall (P<.01) and abstraction ability (P<.05). Stimulant users performed worse on several tests relative to the other drug use groups. Only one of six tests demonstrated improvements following about 3 months of abstinence. Thus, chronic drug use is associated with cognitive impairments that do not improve substantially even after several months of abstinence.

Achievement↗