A novel voltammetric method of local anesthetics such as lidocaine, trimecaine and mepivacaine determination has been developed. The proposed method was based on the obtaining of anesthetic N‐oxides in oxidation reaction with futher reduction of reaction product. Experimental conditions affecting quantitative yield of anesthetic N‐oxides such as oxidation time, oxidant concentration and temperature were studied. This assay was found to be linear (R=0.999) over a concentration range n⋅10−6–5 ⋅ 10−5 mol L−1. Calculated LOD and LOQ were found to be 0.38 and 1.14 μg mL−1 respectively. Sensitivity of presented method is comparable with that of chromatographic method. Overall, the developed method exhibited good selectivity towards components of pharmaceuticals and biological fluids. The proposed method was successfully applied to the analysis of studied anesthetics in different pharmaceutical samples.
Biologically active compounds containing sulfhydryl groups (RSHs: N-acetyl-Lcysteine, D-penicillamine, glutathione and acetylthiocholine chloride) were used to develop a luminometric method for their quantification. The title substrate capable of chemiluminescence (CL) was isolated in a highly pure state as a chloride salt (99.9% using RP-HPLC) and identified using mass spectrometry (ESI Q-TOF) and 1 H NMR spectroscopy. The cation included in the salt, 9-CMA + , underwent oxidation in an alkaline environment containing RSHs by molecular oxygen, generating CL of various intensities, with no need for the use of hydrogen peroxide. The amount of produced light was linearly proportional to the content of investigated analytes in the system over the concentration range $0.2-2 μM, with the detection limits in the range 0.19-1.73 μM. The mechanism of chemiluminogenic oxidation of 9-CMA + in the
A new polarographic method for the determination of benzocaine and procaine based on the polarographic reduction of their chemically obtained oxidation products with potassium peroxymonosulfate is developed. Experimental conditions affecting quantitative yield of benzocaine and procaine oxidation products such as рH, oxidation time, reagents’ concentration, and temperature are explored. It is shown that the reduction current changes in a linear fashion (R=0.999) with increasing concentration of anesthetics over a concentration range of 1·10−6 - 5·10−5 mol L−1. The calculated limits of detection (LOD) for benzocaine and procaine are found to be 5.6·10−6 and 6·10−6 mol L−1, respectively. In the present study, quantitative polarographic determination of benzocaine in Farisil tablets and “Septolete Plus” lozenges and procaine in solution for injections is performed. The results of the analysis are in good agreement with the product specifications described in the quality certificates. The possibility of quantitative determination of benzocaine and procaine in pharmaceuticals is confirmed.
In the article the results of the study of toxic effect of the designed disinfectant (active ingredient potassium peroxomonosulfate) on laboratory animals (mice) are presented. For the recent years a variety of scientific works both by domestic and by foreign scientists has been devoted to the study of different disinfectants’ toxicity. However today there is a number of issues that require more detailed studying and scientific justification. Among them the problem of toxic effects of disinfectants on the animal organism occupies a special place. The aim of our work was to study the toxic effect on the laboratory animals and to assess the acute toxicity (LD50) of the designed ‘Bondarmin’ disinfectant. Tests were carried out at the Laboratory of pharmacology and toxicology of the National University of Pharmacy (Kharkiv) and on the base of Educational and scientific laboratory of genetic and molecular research methods named after P. I. Verbitskiy in the Kharkiv State Zooveterinary Academy. Acute toxicity assessment (LD50) was carried out with intragastrointestinal administration of the designed drug to laboratory animals (mice). Changes in the internal organs of animals that were removed from the experiment for humane reasons and those who died after the experiment were detected by macroscopic examination. The lethality of laboratory animals after the intragastric administration of disinfectant was determined by the Prozorovskiy method The dynamic of changes in body weight of mice after the administration of disinfectant in high doses (from 1,500 to 3,500 mg/kg) was found out. The influence of the disinfectant on the mass coefficients of the internal organs of male mice after intragastric administration was evaluated. Toxic effect of the designed disinfectant ‘Bondarmin’, when using intragastric method of administration to laboratory animals (mice), according to the age and sexual index (LD50 = 2,702.40 ± 156.32 mg/kg), was established. Disinfectant ‘Bondarmin’ refers to IV toxicity class (low toxic substances).
In present paper we described a new simple voltammetric method of determination of nefopam alkaloid and its metabolite – N‐oxide. N‐oxide of nefopam is reduced at the dropping mercury electrode (DME) and silver solid amalgam electrodes (AgSAE), which can effectively replace mercury and chemically modified electrodes. The reduction consists of two one‐electron stages each accompanied with one proton transfer. N‐oxide of nefopam can be obtained from nefopam substance by oxidation with potassium peroxymonosulfate. It was studied the effect of various factors on N‐oxide quantitative yield (pH, oxidation duration, reagents concentration) as well as on the reduction of N‐oxide at DME and p‐AgSAE (pH, the nature of background electrolyte, potential and time of accumulation). It was showed that the reduction current linearly increased with increasing of concentration of analgesic. Limit of quantiation is 10−6 mol L−1 at DME and 10−7 mol L−1 at p‐AgSAE. The developed method was applied for the analysis of commercial drug solution for injection “Nefopam” with recovery of 96.7 %, as well as for the spiked human urine samples. Excellent repeatability with a relative standard deviation below 5 % was achieved.
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