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Objective: The aim of this study was to evaluate the reliability of a non-invasive method (saliva) for determination of testosterone level in diagnosing cases of Polycystic Ovarian Syndrome (PCOS), and comparing it with serum free testosterone. Study design: Prospective clinical controlled trial. Participants and interventions: Fifty women with PCOS and 20 normal women as control group were selected for the study. They all aged between 23 and 35year. For all patients serum follicle stimulating hormone (FSH) and luteinizing hormone (LH) were assessed by chemiluminescent assay. Serum free testosterone (FT) was assayed by radioimmunoassay (RIA) and salivary testosterone (ST) by ELISA technique. BMI was calculated for all participants and transvaginal sonography to determine ovarian morphology and ovarian volume. Results: The present study showed a significant positive correlation between salivary testosterone, as measured by ELISA, and serum free testosterone measured by RIA (p=0.001 and r=0.52). Using the receiver operator curve, salivary testosterone was found to be more sensitive than serum (FT) (84% vs. 66%) in diagnosing PCOS patients. Conclusion: Determination of salivary testosterone is a reliable method to detect changes in the concentration of available biologically active testosterone in the serum. Salivary testosterone provides a sensitive, simple, reliable, non-invasive and uncomplicated diagnostic approach for PCOS.

To evaluate the reproductive and metabolic effects of L-carnitine plus metformin in clomiphene citrate (CC) resistant obese polycystic ovary syndrome (PCOS) women. A double-blinded randomized controlled clinical trial, clomiphene-citrate resistant obese women were allocated randomly to receive CC plus metformin and L-carnitine ( n  = 138) or CC plus metformin and placebo ( n  = 136). The primary outcome was clinical pregnancy rate. The secondary outcomes were hormonal and metabolic profile changes in addition to ovulation and first trimester (13 weeks) miscarriage rates. Clomiphene-citrate, L-carnitine, and metformin group showed significant improvement in the menstrual regularity, ovulation rate, and pregnancy rate compared to CC plus metformin and placebo group (29% vs. 9%, 34.7% vs. 11%, and 28.2% vs. 6.6%, respectively). No statistically significant difference in the miscarriage rate between the two groups ( p  = .08). After three months of treatment, the reduction in body mass index (BMI) was non-significant ( p  = .061) between both groups. The hormonal and metabolic parameters were more significantly improved in the L-carnitine group compared with the placebo group. l-Carnitine may act synergistically with metformin for improvement of reproductive performance, insulin resistance, and lipid profile in clomiphene-resistant obese PCOS women.

A highly sensitive, simple and rapid spectrofluorimetric method was developed for the determination of lacidipine (LCP) in tablets. The proposed method is based on the investigation of the fluorescence spectral behavior of LCP in both sodium dodecyl sulphate (SDS) and the tween-80 micellar system. In aqueous solutions of acetate buffer (pH 4.5), the fluorescence intensities of LCP were greatly enhanced (ca. 2.4 and 4.3 folds) in the presence of either SDS or tween-80, respectively. The fluorescence intensity was measured at 444 nm after excitation at 277 nm using either SDS or tween-80 as a surfactant. The fluorescence-concentration plots were rectilinear over the ranges of 50.0-500.0 ng/ml and 5.0-200.0 ng/ml with lower detection limits of 5.11 and 2.06 ng/ml and lower quantification limits of 17 and 6.87 ng/ml using SDS and tween-80, respectively. The method was successfully applied to the analysis of LCP in commercial tablets and the results were in good agreement with those obtained with the comparison method. Furthermore, content uniformity testing of pharmaceutical tablets was also conducted., (Copyright © 2014 John Wiley & Sons, Ltd.)

A simple, sensitive and rapid spectrofluorimetric method was developed for the determination of esomeprazole (EMZ) and pantoprazole (PRZ) in their pharmaceutical formulations and human plasma. The proposed method is based on the fluorescence spectral behavior of EMZ in methanol in the presence of 0.1 m NaOH containing 0.5% methyl cellulose (MC) at 306/345 nm. The fluorescence intensity of EMZ was enhanced about 1.3-fold and good linearity in the range 0.4-4.0 µg/mL with a lower detection limit of 0.04 µg/mL and lower quantification limit of 0.14 µg/mL. For PRZ, its methanolic solution exhibited marked native fluorescence at 290/325 nm after enhancement (about 2.1- or 1.4-fold) using either 0.025% sodium dodecyl sulfate (SDS) or 0.05% MC in the presence of 0.2 m borate buffer of pH 9.5. The fluorescence-concentration plots of PRZ were rectilinear over the ranges 0.2-2.0 and 0.3-3.0 µg/mL with lower detection limits of 0.02 and 0.03 µg/mL and lower quantification limits of 0.07 and 0.09 µg/mL using sodium dodecyl sulfate and MC, respectively. The method was successfully applied to the analysis of EMZ and PRZ in their commercial dosage forms and the results were in good agreement with those obtained with the comparison method. Furthermore, in a preliminary investigation, the proposed method was extended to the in vitro determination of the two drugs in spiked human plasma and the results were satisfactory., (Copyright © 2014 John Wiley & Sons, Ltd.)

Two sensitive fluorometric methods were developed for the determination of both bopindolol malonate (BOP) and celiprolol HCl (CLP) based on measuring their native fluorescence in methanol and acetonitrile, respectively. For BOP, the fluorescence was measured at 316 nm after excitation at 278 nm. The proposed method was successfully applied to the assay of commercial tablets as well as content uniformity testing. For CLP, the fluorescence was enhanced by the addition of carboxymethylcellulose solution and measured at 455 nm after excitation at 339 nm. The method was successfully applied to the analysis of CLP in tablets and biological fluids. In both methods, interference likely to be introduced from co-formulated, co-administered, or chemically related drugs was studied. The results were statistically compared with those obtained by reference methods and were found to be in good agreement.

A rapid, simple and highly sensitive first derivative synchronous fluorometric method has been developed for the simultaneous analysis of binary mixture of sulpiride (SUL) and mebeverine hydrochloride (MEB). The method is based upon measurement of the synchronous fluorescence intensity of these drugs at ∆λ = 100 nm in water. The different experimental parameters affecting the fluorescence of the two drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.05-1 µg/mL and 0.2-3.2 µg/mL for SUL and MEB respectively with lower detection limits (LOD) of 0.006 and 0.01 µg/mL and quantification limits (LOQ) of 0.0.02 and 0.05 µg/mL for SUL and MEB, respectively. The proposed method was successfully applied for the determination of the two compounds in synthetic mixtures and in commercial tablets. The high sensitivity attained by the proposed method allowed the determination of both of SUL and MEB metabolite (veratic acid) in real human plasma samples applying second derivative synchronous fluorometric technique. The mean% recoveries (n = 3) for both MEB metabolite (veratic acid) and SUL were 99.82 ± 2.53 and 98.84 ± 6.20 for spiked human plasma respectively, while for real human plasma, the mean% recoveries (n = 3) were 91.49 ± 4.25 and 91.36 ± 8.46 respectively.

Two Spectrophotometric procedures are presented for the determination of two commonly used H2-receptor antagonists, nizatidine (I) and ranitidine hydrochloride (II). The methods are based mainly on charge transfer complexation reaction of these drugs with either p-chloranilic acid (rho-CA) or 2, 3 dichloro-5, 6-dicyanoquinone (DDQ). The produced colored products are quantified spectrophotometrically at 515 and 467 nm in chloranilic acid and DDQ methods, respectively. The molar ratios for the reaction products and the optimum assay conditions were studied. The methods determine the cited drugs in concentration ranges of 20-200 and 20-160 microg/mL for nizatidine and ranges of 20-240 and 20-140 microg/mL for ranitidine with chloranilic acid and DDQ methods, respectively. A more detailed investigation of the complexes formed was made with respect to their composition, association constant, molar absorptivity and free energy change. The proposed procedures were successfully utilized in the determination of the drugs in pharmaceutical preparations. The standard addition method was applied by adding nizatidine and ranitidine to the previously analyzed tablets or capsules. The recovery of each drug was calculated by comparing the concentration obtained from the spiked mixtures with those of the pure drug. The results of analysis of commercial tablets and the recovery study (standard addition method) of the cited drugs suggested that there is no interference from any excipients, which are present in tablets or capsules. Statistical comparison of the results was performed with regard to accuracy and precision using student's t-test and F-ratio at 95% confidence level. There is no significant difference between the reported and proposed methods with regard to accuracy and precision.

A sensitive and rapid spectrophotometric procedure has been investigated for the determination of fenoterol either per se or in pharmaceutical preparations. The proposed procedure is based on the reaction between the drug and 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) at pH 7.2, using borate buffer, to produce a yellow adduct. The latter has maximum absorbance at 400 nm and obeys Beer's law within the concentration range 5-30 microg/ml. Regression analysis of the calibration data showed a good correlation coefficient (r=0.9996) with minimum detection limit of 0.24 microg/ml (6.2 x 10(-8) M). The proposed procedure has been successfully applied to the determination of this drug in its tablets and in syrup, the mean percent recoveries were 97.45+/-0.59 and 98.7+/-0.64%, respectively. The results obtained are in good agreement with those given using a reference method. The pharmaceutical additives other than active ingredient did not interfere. A proposal of the reaction pathway has been postulated.

The kinetics of the uptake of Fe(II)-histidinate, a known promoter of lipid peroxidation, into Ehrlich ascites tumor (EAT) cells and the intracellular binding of iron were studied in vitro. EAT cells (27.10(6)/ml) were incubated in Hanks' balanced salts solution at 37 degrees C for various time intervals in the presence of FeSO4 (1 mM) and L-histidine (10 mM). Total iron was determined by the 1,10-phenanthroline/ascorbate method and ferric iron by reaction with 5-sulfosalicylic acid; the difference was ascribed to ferrous iron. Total iron decreased rapidly in the medium (242 nmol within the first 10 min), and a corresponding increase of total iron (saturation value 376 nmol after 60 min) was determined within the cells, after the cellular proteins had been solubilized with 6 M urea. In the absence of EAT cells, Fe(II)-histidinate was readily oxidized to Fe(III)-histidinate by oxygen, but this reaction was strongly retarded by the tumor cells. The uptake of iron histidinate occurred in the oxidized state, while an uptake of ferrous iron could not be proven unambiguously. When EAT cells were saturated with iron, it was found that 93% of intracellular iron was bound to water-insoluble proteins and 7% was associated with soluble proteins, while no unbound iron was detectable by the method used. It was concluded that, despite the high uptake of total iron, only a very small portion of the intracellular iron was available as a redox catalyst for lipid peroxidation.

A simple and selective spectrophotometric method for the determination of some pharmaceutically important nitro compounds has been developed. The suggested method depends upon the spectral changes induced by reduction using either Zn/HCl or Zn/NH4Cl. The different experimental parameters were studied and incorporated into the procedure. The mean percentage recovery ranged from 99 to 101. The proposed method was applied to the determination of the studied compounds in dosage forms, and the results obtained were compared favourably with those given with the compendial ones.