Comparative effects of different supplemented dietary doses of chlorophyll on blood parameters of experimental male rats.

Chlorophylls are organic pigments that are a part of our daily diet, particularly in light of the increased popularity of more eco-friendly and healthy practices. Since altering oxidative equilibrium seems to be connected to the emergence of numerous illnesses, the antioxidant capacities of both groups of lipophilic compounds have been studied. The objective was to evaluate adding dietary chlorophyll at two concentrations-30 and 60 mg/ml-would improve blood characteristics in rats. Supplemented dietary chlorophyll showed significantly increased WBCs, RBCs, granulocytes, lymphocytes, HGB, HCT MCHC, and Platelets. it nonsignificant effect on RDW, MPV, and Eosinophil. These findings support a significant rise in critical hematological parameters at two separate time intervals, 14 and 28 days following dietary chlorophyll supplementation, at dosages of 30 and 60 mg/ml. After 30 and 60 mg/ml, platelet count, PCT, lymphocytes, and monocytes substantially (p0.001) rose. In light of these findings, critical hematological indicators markedly rise in response to exogenous dietary chlorophyll. To strengthen blood parameters and enhance blood features and prevent anemia, dietary chlorophyll is advised.

DTI of the Olfactory Bulb in COVID-19-Related Anosmia: A Pilot Study.

This study aimed to assess the utility of DTI in the detection of olfactory bulb dysfunction in COVID-19-related anosmia. It was performed in 62 patients with COVID-19-related anosmia and 23 controls. The mean diffusivity and fractional anisotropy were calculated by 2 readers. The difference between the fractional anisotropy and mean diffusivity values of anosmic and control olfactory bulbs was statistically significant (P = .001). The threshold of fractional anisotropy and mean diffusivity to differentiate a diseased from normal olfactory bulb were 0.22 and 1.5, with sensitivities of 84.4% and 96.8%, respectively, and a specificity of 100%.

Polymer complexes. LX. Supramolecular coordination and structures of N(4-(acrylamido)-2-hydroxybenzoic acid) polymer complexes.

A number of novel polymer complexes of various anions of copper(II), cobalt(II), nickel(II) and uranyl(II) with N(4-(acrylamido)-2-hydroxy benzoic acid) (ABH) have been synthesized and characterized by elemental analysis, IR, 1H NMR, magnetic susceptibility measurements, electronic spin resonance, vibrational spectra and thermal analysis. The molecular structures of the ligand are optimized theoretically and the quantum chemical parameters are calculated. Tentative structures for the polymeric metal complexes due to their potential application are also suggested. The IR data exhibit the coordination of ONO2/OAc/SO4 with the metal ions in the polymeric metal complex. Vibrational spectra indicate coordination of carboxylate oxygen and phenolic OH of the ligand giving a MO4 square planar chromophore. Ligand field ESR spectra support square planar geometry around Cu(II). The thermal decomposition of the polymer complexes were discussed in relation to structure, and the thermodynamic parameters of the decomposition stages were evaluated applying Coast-Redfern and Horowitz-Metzger methods.

Optical and thermal properties of azo derivatives of salicylic acid thin films.

N-acryloyl-4-aminosalicylic acid (4-AMSA), monomer (HL) and 5-(4'-alkyl phenylazo)-N-acryloyl-4-aminosalicylic acid (HLn) are synthesized and characterized with various physico-chemical techniques. Thin films of 5-(4'-alkyl phenylazo)-N-acryloyl-4-aminosalicylic acid (HLn) are prepared by spin coating technique. The X-ray diffraction (XRD) patterns of 4-aminosalicylic acid (4-ASA) and its derivatives are investigated in powder and thin film forms. Thermal properties of the compounds are investigated by thermogravemetric analysis (TGA). The optical energy gap and the type of optical transition are investigated in the wavelength range (200-2500 nm) for 4-ASA, HL and HLn. The values of fundamental energy gap (Eg) are in the range 3.60-3.69 eV for all compounds and the type of optical transition is found to be indirect allowed. The onset energy gap Eg(∗) appeared only for azodye compounds is found to be in the range 0.95-1.55 eV depending on the substituent function groups. The refractive index, n, shows a normal dispersion in the wavelength range 650-2500 nm, while shows anomalous dispersion in the wavelength rang 200-650 nm. The dispersion parameters ε∞, εL, Ed, Eo and N/m(∗) are calculated. The photoluminescence phenomena (PL) appear for thin films of 4-ASA and its derivatives show three main emission transitions.

Development of a voltammetric procedure for assay of the antihistamine drug hydroxyzine at a glassy carbon electrode: Quantification and pharmacokinetic studies.

An electrochemical study of hydroxyzine at a glassy carbon electrode was carried out in the Britton-Robinson universal buffer of pH 2-11. Hydroxyzine was oxidized in a single two-electron irreversible process controlled mainly by adsorption. A simple, sensitive and time-saving square-wave adsorptive anodic stripping voltammetric procedure has been developed for determination of hydroxyzine in its commercial tablets and human serum without prior extraction. The optimized procedural conditions were: frequency=120Hz, scan increment=10mV, pulse-amplitude=25mV, accumulation potential=-0.3V, accumulation time=90-300s and a Britton-Robinson universal buffer of pH 4 as a supporting electrolyte. Mean recoveries of 100.5+/-0.71 and 98.6+/-1.12% (n=5) were achieved for assay of hydroxyzine in Atarax 10 and 25mg dosage forms, respectively. Limit of detection of 1.5x10(-8)molL(-1) (5.624ngmL(-1)) and limit of quantitation of 5.0x10(-8)molL(-1) (18.746ngmL(-1)) were achieved in human serum with a mean recovery of 98.4+/-1.22%, without prior extraction of the drug. Moreover, the described procedure was applied for evaluating the pharmacokinetic parameters of hydroxyzine in plasma of two healthy volunteers after administration of a single oral dose (Atarax)-25mg).

Immediate peri-operative memory.

BACKGROUND: Information about anterograde and retrograde amnesias in the immediate peri-operative period is scarce. During this period, assessment of memory for real-life events is also rare. We hypothesized that there would be both anterograde and retrograde amnesias and memory for peri-operative events would be better than for verbal memory. METHODS: We studied 40 patients who underwent general anesthesia and surgery and 19 control volunteers who were matched to the patients but did not have surgery. Patients completed the state anxiety part of the Spielberger State-Trait Anxiety Inventory in the pre-operative period. They were presented with three word lists in the holding area, the operating room before induction of anesthesia and the recovery room. Memory for the words was tested the next day by recall and recognition tests. Memory for events that happened on the day of surgery was tested by administering a questionnaire. The control subjects were tested similarly but did not complete the events questionnaire. Retrograde amnesia would be demonstrated by a decline in patients' memory from the holding area to the operating room which exceeded any corresponding changes in controls; anterograde amnesia would be demonstrated by memory impairment of the patients in the recovery room, relative to controls. RESULTS: Recall and recognition of words were significantly impaired in the recovery room with a decline from 12% in the holding area to zero% in the recovery room for recall and from 43% to 7% for recognition. The decline in memory from the holding area to the operating room was not significantly greater in patients than in controls, 80% vs. 56% for recall and 27% vs. 14% for recognition. There were no significant differences for recognition of events which happened in the three rooms. CONCLUSIONS: We were unable to detect retrograde amnesia. Patients' memory for neutral stimuli in the recovery room was severely impaired. The events questionnaire proved to be insensitive.

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.

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.

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.

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.

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.

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.

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.

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 pH10) 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.

A validated stripping voltammetric procedure for quantification of the anti-hypertensive and benign prostatic hyperplasia drug terazosin in tablets and human serum.

The electrochemical behavior of terazosin at the hanging mercury drop electrode was studied in Britton-Robinson buffer (pH 2-11), acetate buffer (4.5-5.5), and in 0.1M solution of each of sodium sulfate, sodium nitrate, sodium perchlorate and potassium chloride as supporting electrolytes. The square-wave adsorptive cathodic stripping voltammogram of terazosin exhibited a single well-defined two-electron irreversible cathodic peak which may be attributed to the reduction of CO double bond of the drug molecule. A fully validated, simple, high sensitive, precise and inexpensive square-wave adsorptive cathodic stripping voltammetric procedure was described for determination of terazosin in bulk form, tablets and human serum. A mean recovery for 1x10(-8)M terazosin in bulk form, following preconcentration onto the hanging mercury drop electrode for 60s at a -1.0V (versus Ag/AgCl/KCl(s)), of 99+/-0.7% (n=5) was obtained. Limits of detection (LOD) and quantitation (LOQ) of 1.5x10(-11) and 5x10(-11)M bulk terazosin were achieved, respectively. The proposed procedure was successfully applied to determination of the drug in its Itrin((R)) tablets and human serum samples. The achieved LOD and LOQ of the drug in human serum samples were 5.3x10(-11) and 1.8x10(-10)M THD, respectively. The pharmacokinetic parameters of the drug in human plasma were estimated as: C(max)=77.5ngml(-1), t(max)=1.75h, AUC(0-t)=602.3nghml(-1), K(e)=0.088h(-1) and t(1/2)=11.32h) which are favorably compared with those reported in literature.

Voltammetric behavior and assay of the contraceptive drug levonorgestrel in bulk, tablets, and human serum at a mercury electrode.

The cyclic voltammograms of levonorgestrel (LNG) in Britton-Robinson buffers of pH 2-11 at the hanging mercury drop electrode showed a single two-electron irreversible cathodic peak over the whole pH range. This peak may be attributed to the reduction of the 3-keto-delta-4-group in the A-ring of the LNG molecule. The interfacial adsorptive character of levonorgestrel onto the surface of the hanging mercury drop electrode was identified by means of both cyclic voltammetry and chronocoulometry techniques. A simple, sensitive, and selective square-wave adsorptive cathodic stripping voltammetric procedure was developed for the quantitation of levonorgestrel. Under the optimized operational conditions, the maximum developed stripping voltammetric peak current showed a linear response with concentration of the bulk LNG substance. The achieved limits of detection (LOD) and quantitation (LOQ) were 6.7x10(-10) and 2.2x10(-9)M, or 4.8x10(-10) and 1.6x10(-9)M, following accumulation onto the hanging mercury drop electrode for 90s or 150s, respectively. The developed procedure was successfully applied to the determination of levonorgestrel in tablets, in spiked human serum, and in real plasma samples of healthy female volunteers following an oral administration of a 30-mug LNG single dose. The pharmacokinetic parameters (C(max)=1.05ngml(-1), t(max)=2.4h and AUC(0-t)=16.5nghml(-1)) were estimated and favorably compared to those reported in literature for equivalent dose.

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.

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.

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).

Adsorptive stripping voltammetric determination of the anti-inflammatory drug celecoxib in pharmaceutical formulation and human serum.

Celecoxib is a cyclooxygenase inhibitor, that has been recently and intensively prescribed as an anti-inflammatory drug in rheumatic osteoarthritis. A robust, highly reliable and reproducible square-wave (SW) adsorptive cathodic stripping voltammetric procedure was developed for the determination of celecoxib in pharmaceutical formulation and human serum. The analytical procedure was based on the reduction of the CN of the pyrazole ring of the drug molecule at the mercury electrode surface in Britton-Robinson buffer of pH 7.0. The SW adsorptive cathodic stripping voltammogram of celecoxib showed a single well-defined peak at -1.54 V (vs. Ag/AgCl/KCl(s)) using an accumulation potential of -0.70 V, frequency of 120 Hz, scan increment of 10 mV and pulse amplitude of 25 mV. Repeatability was examined for 1 x 10(-8) M CXB drug solution after 30 s pre-concentration and a mean recovery of 99.4+/-0.4% (n=5) was achieved. For 90 s preconcentration, a linear concentration range of 1 x 10(-9)-2 x 10(-8) M CXB and a detection limit of 1.86 x 10(-10) M were achieved. The proposed procedure was successfully applied for the determination of the drug in capsules and human serum with mean recoveries of 101.5+/-0.6 and 98.8+/-1.1%, respectively. A detection and quantitation limits of 1.0 x 10(-9) M (0.4 ng ml(-1)) and 4.7 x 10(-9) M (1.3 ng ml(-1)) were achieved for the determination of the drug in human serum. Moreover, the procedure was useful for study of the pharmacokinetic profile of celecoxib in a healthy volunteer after administration of a single oral dose (celebrex, 200 mg).