Complexation of some trivalent lanthanides, scandium(III) and thorium(IV) by benzylidenepyruvates and cinnamylidenepyruvate in aqueous solution

The protonation constants of benzylidenepyruvate, 2-chloro-, 4-chlorobenzylidinepyruvate and cinnamylidenepyruvate as well as the stability constants of their binary 1:1 complexes with Cu(II), La(III), Pr(III), Sm(III), Lu(III), Sc(III) and Th(IV) have been determined spectrophotometrically in an aqueous medium at 25 °C and ionic strength 0.500 M, held with sodium perchlorate. Coordination centres in the aforementioned ligands are suggested. © 1995.

In vitro effect of sodium trimetaphosphate additives to conventional toothpastes on enamel demineralization

The aim of this study was to evaluate the ability of conventional toothpastes (1100 ppm F) supplemented with sodium trimetaphosphate (TMP) in demineralization. Blocks of enamel were selected and then divided into seven experimental groups of 12: toothpaste without F and TMP (placebo), toothpaste with 1100 ppm F (1100), and toothpaste with 1100 ppm F supplemented with TMP-1 % (1100 1 % TMP), 3 % (1100 3 % TMP), 4.5 % (1100 4.5 % TMP), 6 % (1100 6 % TMP), and 9 % (1100 9 % TMP). Blocks were subjected to five pH cycles (demineralizing/remineralizing solutions) at 37 °C and treated with toothpaste slurries twice daily, after which the blocks were maintained for 2 days in fresh remineralizing solution. Following treatments, surface hardness (SHf) and cross-sectional hardness were determined for calculating the integrated loss of subsurface hardness (ΔKHN). The fluoride present in the enamel was also measured. The SHf and ΔKHN measurements showed that supplementation with 3 % TMP was the most effective (p < 0.001) and showed greater concentration of F in the enamel (p < 0.001). Addition of 3 % TMP to a conventional toothpaste (1100 ppm F) showed greater efficacy in reducing enamel demineralization. Fluoride toothpastes containing trimetaphosphate possess good anticaries potential required to reduce the prevalence of dental caries in high-risk patients.

Synergistic effect of fluoride and sodium hexametaphosphate in toothpaste on enamel demineralization in situ

To evaluate the effect of a fluoride dentifrice containing sodium hexametaphosphate (HMP) on enamel demineralization in situ. This double-blind and cross-over study consisted of 3 phases (7 days each) in which 12 volunteers wore intraoral appliances containing four enamel bovine blocks. Specimens were treated (3×/day) with placebo (no F or HMP), 1100ppm F (1100F) and 1100F plus HMP1% (1100F-HMP1%) toothpastes, and the cariogenic challenge was performed using a 30% sucrose solution (6×/day). Final surface hardness, the percentage of surface hardness loss (%SH), the integrated loss of subsurface hardness (ΔKHN), as well as enamel calcium (Ca), phosphorus (P) and firmly-bound fluoride (F) were determined. Also, biofilm formed on the blocks were analyzed for F, Ca, P and insoluble extracellular polysaccharide (EPS) concentrations. Data were submitted 1-way ANOVA, followed by Student-Newman-Keuls' test (p<0.05). 1100F-HMP1% promoted the lowest %SH and ΔKHN among all groups (p<0.001). The addition of HMP1% to 1100F did not enhance enamel F uptake, but significantly increased enamel Ca concentrations (p<0.001). Similar EPS concentrations were seen for 1100F-HMP1% and 1100F groups (p>0.05). All the groups were supersaturated with respect to HA. However, only 1100F-HMP1% group was supersaturated with respect to CaF2 (p<0.05). The ionic activities of F(-), CaF(+) and HF(0) for the 1100F-HMP1% group were the highest among all groups (p<0.001). The addition of HMP1% to a conventional toothpaste significantly reduces enamel demineralization in situ when compared to 1100F. This dentifrice could be a viable alternative to patients at high risk of caries.

Adjuvant therapy with sodium alendronate for the treatment of experimental periodontitis in rats

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Validation of analytical methodology for quantification of cefazolin sodium by liquid chromatography

A reversed-phase high performance liquid chromatography method was validated for the determination of cefazolin sodium in lyophilized powder for solution for injection to be applied for quality control in pharmaceutical industry. The liquid chromatography method was conducted on a Zorbax Eclipse Plus C18 column (250 x 4.6 mm, 5 μm), maintained at room temperature. The mobile phase consisted of purified water: acetonitrile (60: 40 v/v), adjusted to pH 8 with triethylamine. The flow rate was of 0.5 mL min-1 and effluents were monitored at 270 nm. The retention time for cefazolin sodium was 3.6 min. The method proved to be linear (r2 =0.9999) over the concentration range of 30-80 µg mL-1. The selectivity of the method was proven through degradation studies. The method demonstrated satisfactory results for precision, accuracy, limits of detection and quantitation. The robustness of this method was evaluated using the Plackett–Burman fractional factorial experimental design with a matrix of 15 experiments and the statistical treatment proposed by Youden and Steiner. Finally, the proposed method could be also an advantageous option for the analysis of cefazolin sodium, contributing to improve the quality control and to assure the therapeutic efficacy

Development and validation of an economic, environmental friendly and stability-indicating analytical method for determination of ampicillin sodium for injection by RP-HPLC

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development of an innovative, ecological and stability-indicating analytical method for semiquantitative analysis of ampicillin sodium for injection by thin layer chromatography (TLC)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Spectrophotometric determination of ciprofloxacin hydrochloride in ophthalmic solution

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development and validation of a stability-indicative agar diffusion assay to determine the potency of flucloxacillin sodium in capsules

Flucloxacillin sodium (FLU) is a semi-synthetic penicillin active against many gram-positive bacteria such as streptococci and penicilinase-producing staphylococci, including methicillin-susceptible S. aureus. This study describes the development and validation of a microbiological assay, applying the diffusion agar method for the determination of FLU, as well as the evaluation of the ability of the method in determining the stability of FLU in capsules against acidic and basic hydrolysis, photolytic and oxidative degradations, using S. aureus ATCC 25923 as micro-organism test and 3 x 3 parallel line assay design (three doses of the standard and three doses of the sample in each plate), with six plates for each assay, according to the Brazilian Pharmacopoeia. The validation method showed good results including linearity, precision, accuracy, robustness and selectivity. The assay is based on the inhibitory effect of FLU using Staphylococcus aureus ATCC 25923. The results of the assay were treated by analysis of variance (ANOVA) and were found to be linear (r = 0.9997) in the range from 1.5 to 6.0 μg/mL, precise (repeatability: R.S.D. = 1.63 and intermediate precision: R.S.D. = 1.64) and accurate (98.96%). FLU solution (from the capsules) exposed to direct UVC light (254 nm), alkaline and acid hydrolysis and hydrogen peroxide causing oxidation were used to evaluate the specificity of the bioassay. Comparison of bioassay and liquid chromatography by ANOVA showed no difference between methodologies. The results demonstrated the validity of the proposed bioassay, which is a simple and useful alternative methodology for FLU determination in routine quality control.

Validation of cefazolin sodium by UV-spectrophotometric method

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Methods for qualitative analysis of cefazolin sodium raw material and pharmaceutical product

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)