{"title":"Post mortem changes: challenges in drug analysis in the diagnosis of deaths from intoxication","authors":"Marina Camargo Galera, L. G. Rossato-Grando","doi":"10.22456/2527-2616.111711","DOIUrl":"https://doi.org/10.22456/2527-2616.111711","url":null,"abstract":"In forensic toxicology, alternative matrices and sampling sites are required for a correlation of antemortem and postmortem concentrations with the least possible error. Postmortem redistribution phenomena and biochemical changes inherent to these processes are possible, and represent interferences in these analyses. This study aimed to perform a bibliographic review through Pubmed database within a 10-year period of time, using the keywords: forensic analysis AND redistribution. We observed that for quantitative analyses the preferred matrix is blood from peripheral vessels, and when it is not available, vitreous humor is a great specimen for choice. ","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76209113","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Mikaelly Pereira Caet, Millena Almeida Monsores, A. K. M. S. Machado, T. Barth, M. S. Sangoi, V. Todeschini
{"title":"Pharmacopoeial HPLC methodology improvement: A case study of piroxicam","authors":"Mikaelly Pereira Caet, Millena Almeida Monsores, A. K. M. S. Machado, T. Barth, M. S. Sangoi, V. Todeschini","doi":"10.22456/2527-2616.108512","DOIUrl":"https://doi.org/10.22456/2527-2616.108512","url":null,"abstract":"In the present study, a simple, stability-indicating and cost-effective reversed-phase high performance liquid chromatography (HPLC) method was developed and validated for the determination of piroxicam in commercial and masterful formulation capsules as an alternative to existing methods. The improved HPLC method was carried out on a C18 column (150 mm x 4.6 mm i.d., 5 μm), maintained at 30 °C. The mobile-phase consisted of a solution of triethylamine 0.3% pH 5.0 and acetonitrile (70:30; v/v), run at a flow rate of 1.0 mL/min and using photodiode array (PDA) detection at 248 nm. The chromatographic separation is obtained with retention time of 6.8 min, presenting adequate system suitability parameters for HPLC analysis. Validation parameters such as the specificity, linearity, matrix effect, precision, accuracy and robustness were evaluated in accordance with the ICH Q2(R1) and Brazil RDC 166/17 requirements, giving satisfactory results within the acceptable range. The proposed method was successfully validated and applied for piroxicam analysis, contributing to improve the quality control, and can be used as easy, accurate, low time-consuming alternative to pharmacopeial quantification methodology of drug.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2020-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82603599","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Emeli Araújo, L. Romeiro, Anabela S Rodrigues, P. Alves, V. D. Silva, L. P. L. Logrado, Maria Lucília dos Santos, M. M. Murta, A. C. Leitāo, Sheila Garcia, G. Dellamora-Ortiz
{"title":"Novel ultraviolet absorbers derived from cashew nut shell liquid: spectrophotometric, in silico and in vitro assays","authors":"Emeli Araújo, L. Romeiro, Anabela S Rodrigues, P. Alves, V. D. Silva, L. P. L. Logrado, Maria Lucília dos Santos, M. M. Murta, A. C. Leitāo, Sheila Garcia, G. Dellamora-Ortiz","doi":"10.22456/2527-2616.108405","DOIUrl":"https://doi.org/10.22456/2527-2616.108405","url":null,"abstract":"The cashew nut shell liquid (CNSL) constituents were isolated by our group leading to four mixtures and seventeen pure compounds, which had chromophoric groups similar to organic ultraviolet (UV) absorbers. In addition, C15 and C8 CNSL-derivatives molecules were rationally planned as UV absorbers. Mixtures and isolated CNSL compounds were demonstrated to be non-phototoxic when evaluated in a phototoxicity assay using the yeast Saccharomyces cerevisiae. Considering the absorption values on the UV range, 6 compounds showed appropriate SPF values regarding the spectrophotometric test. Additionally, in silico and in vitro evaluations were performed, showing non-oral bioavailability, as well as non-mutagenic, non-genotoxic and non-phototoxic properties for the tested compounds. These results contribute favorably to the aimed use of the compounds under analysis as novel organic UV absorbers that have as precursor the phenolic lipid component of CNSL, a waste product obtained as the by-product of cashew nut food processing.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2020-12-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87850173","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Juliana Veloso Ferreira, G. A. Pianetti, C. Fernandes
{"title":"BIOANALYTICAL METHOD BY COLUMN-SWITCHING WITH DIRECT INJECTION OF HUMAN PLASMA FOR DETERMINATION OF SULPHONYLUREAS","authors":"Juliana Veloso Ferreira, G. A. Pianetti, C. Fernandes","doi":"10.22456/2527-2616.91542","DOIUrl":"https://doi.org/10.22456/2527-2616.91542","url":null,"abstract":"Sulphonylureas are widely used in the treatment of Diabetes mellitus, one of the main causes of death in human population. Their determination is essential in pharmacological research and in the development of new drugs. Generally, determination of sulphonylureas in biological matrices is performed using conventional sample preparation techniques, which frequently leads to an increase of analysis time and errors. In this context, a bioanalytical method for the simultaneous determination of sulphonylureas by direct injection of human plasma was developed and optimized. An automated column-switching high performance liquid chromatographic system with a restricted access media (RAM) column coupled to a fused-core column was employed. At the first dimension, a RAM column with mobile phase of ultrapure water pH 6.0 at a flow-rate of 1.0 mL min-1 was used. The valve switching time was 3 minutes. At the second dimension, a C18 guard-column coupled to a C18 fused core column with mobile phase of acetonitrile and 10 mM phosphate buffer pH 3.0 (54:46 v/v) at a flow-rate of 0.8 mL min-1 were employed. The column switching system was performed in backflush configuration with an analyte elution time of 1 minute. Flufenamic acid was used as the internal standard. The mean plasma protein exclusion percentage by the RAM-column was 104.5%. The developed and optimized method showed to be fast and simple, allowing the direct injection of biological sample into the chromatographic system and the simultaneous determination of three sulphonylureas in only 12 minutes, including the sample treatment, separation and detection.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80080293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
E. Flores, F. Duarte, Gabriel T. Druzian, Mariele S. Nascimento, J. Barin, R. Bolzan
{"title":"FEASIBILITY OF DIRECT SOLID SAMPLING FOR ARSENIC DETERMINATION IN SULFUR-CONTAINING ACTIVE PHARMACEUTICAL INGREDIENTS BY GF AAS","authors":"E. Flores, F. Duarte, Gabriel T. Druzian, Mariele S. Nascimento, J. Barin, R. Bolzan","doi":"10.22456/2527-2616.89766","DOIUrl":"https://doi.org/10.22456/2527-2616.89766","url":null,"abstract":"A method for As determination in sulfur-containing active pharmaceutical ingredients (SC-APIs) by direct solid sampling graphite furnace atomic absorption (DSS-GF AAS) was developed. The proposed method was successfully applied to three SC-APIs (hydrochlorothiazide, furosemide and sulfadiazine). Palladium was used as chemical modifier as well as hydrogen during the pyrolysis allowing the direct determination of As in the SC-APIs without interferences caused by gaseous sulfur species. Sample masses (hydrochlorothiazide) from 0.4 to 3 mg were used and calibration with aqueous standard solutions was feasible. The limit of quantification was 0.033 mg g-1 and the calibration ranged from 0.1 to 1.6 ng As. Recoveries for As solutions added directly to the solid samples were between 95 and 103%, showing a good accuracy. The method validation highlighted its robustness, since variation in pyrolysis and atomization temperatures, as well as in Pd and sample masses, did not change significantly the results. Additional experiments showed that this method can be applied to other SC-APIs (as e.g., furosemide and sulfadiazine). Arsenic concentration in hydrochlorothiazide samples ranged from 0.13 to 0.48 mg g-1, while in furosemide and sulfadiazine samples it was from 0.49 and 0.54 mg g-1, respectively. The use of DSS-GF AAS does not require previous sample digestion and As could be directly determined in the solid samples providing some advantages, as lower risks of contamination and analyte losses, good accuracy and limits of quantification.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88484186","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
R. Cé, D. S. Jornada, J. G. D. Marchi, S. Guterres, A. Pohlmann
{"title":"DRY-POWDER OF CHITOSAN-COATED LIPID-CORE NANOCAPSULES CONTAINING DAPSONE: DEVELOPMENT, LASER DIFFRACTION CHARACTERIZATION AND ANALYTICAL QUANTIFICATION","authors":"R. Cé, D. S. Jornada, J. G. D. Marchi, S. Guterres, A. Pohlmann","doi":"10.22456/2527-2616.92750","DOIUrl":"https://doi.org/10.22456/2527-2616.92750","url":null,"abstract":"Analytical techniques are critical for ensuring physical and chemical stability of a drug both for assessing the stability of drug molecules and for quantifying and identifying the drug content in products. We proposed the development of dry-powders of lipid-core nanocapsules containing dapsone and coated with chitosan, as well as, the analytical quantification of dapsone in dry-powders with 1% and 2% (m/v) of leucine by high-performance liquid chromatography (HPLC). Size is the most relevant physicochemical property of nanoparticulated drug delivery systems. In this context, our results demonstrated that during the powders redispersion in water, could be observed that the mean particle diameters (DAP-LNC-CS-L1 and DAP-LNC-CS-L2) decreased with redispersion times increase. The spray-drying of the lipid-core nanocapsule formulations showed yields ranging from 58 ± 1.0 % (DAP-LNC-CS-L1) to 61 ± 1.5 % (DAP-LNC-CS-L2) indicating an efficient drying process. In this context, the analytical quantifications of dapsone in the dry powders of nanocapsules by HPLC showed that the dapsone content ranged from 92 ± 1.4% (DAP-LNC-CS-L2) to 95 ± 0.8% (DAP-LNC-CS-L1). Can be concluded that spray-drying process of DAP-LNC-CS-L1 and DAP-LNC-CS-L2 formulations showed an efficient aqueous dispersion of nanocapsule powders and the analytical quantification of dapsone in spray-dryed powders were higher than 90%.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89193547","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Ayres, S. Campanharo, E. Schapoval, Nathalie R. Wingert, M. Steppe
{"title":"EVALUATION OF THE STABILITY OF VIGABATRIN IN HOSPITALAR EXTEMPORANEOUS FORMULATIONS","authors":"M. Ayres, S. Campanharo, E. Schapoval, Nathalie R. Wingert, M. Steppe","doi":"10.22456/2527-2616.94436","DOIUrl":"https://doi.org/10.22456/2527-2616.94436","url":null,"abstract":"The aim of this study was to analyze the chemical stability of the anticonvulsant vigabatrin extemporaneous formulation from tablets in storage conditions of different temperatures and types of packaging used. The analysis of vigabatrin extemporaneous formulations were performed by high-performance liquid chromatography (HPLC). The method described in British Pharmacopoeia was co-validated for specificity, linearity, precision and accuracy. Vigabatrin extemporaneous solutions were prepared in triplicate and placed in amber glass and PET bottles, which were stored under three different conditions: at room temperature (15 to 30 °C), under refrigeration (2 to 8 °C), and oven (40 °C). Samples of solutions stored at room temperature and refrigeration were collected every 7 days along 35 days. The same was done for solutions kept at 40 °C, but for a period of 28 days. It was also analyzed the solutions pH in each sampling time. Vigabatrin extemporaneous solutions showed variations within the limits of British Pharmacopoeia 2016 up to 21 days in amber PET and glass bottles at room and refrigerated temperatures. Vigabatrin content for formulations kept in oven decreased above 10% after 7 days of study. The lowest pH change occurred in amber glass bottle stored under refrigeration. Results of this study will be applied as a reference for vigabatrin extemporaneous formulation in hospital, once it was demonstrated the reliability of storage time interval and proper conditions for the use. Thus, pediatric patients with fractionated doses or use of nasogastric probe will have adequately prepared extemporaneous formulations, reducing the risk of dilution errors and microbiological contamination, improving the efficacy and safety, and enabling more time for nursing assistance. ","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87099760","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
J. Sorrentino, R. Sponchiado, Natália O. dos Santos, S. S. Oliveira, K. Galle, C. V. Garcia, A. Fuentefria, M. Steppe
{"title":"BIOTRANSFORMATION OF METRONIDAZOLE BY CUNNINGHAMELLA ELEGANS ATCC 9245","authors":"J. Sorrentino, R. Sponchiado, Natália O. dos Santos, S. S. Oliveira, K. Galle, C. V. Garcia, A. Fuentefria, M. Steppe","doi":"10.22456/2527-2616.94032","DOIUrl":"https://doi.org/10.22456/2527-2616.94032","url":null,"abstract":"Drug biotransformation studies appear as an alternative to pharmacological studies of metabolites, development of new drug candidates with reduced investment as well as the most efficient production of chemical structures involves and drug quality control studies. A wide range of reactions in biotransformations process is catalyzed by microorganisms. Fungi can be considered as a promising source of new biotransformation reactions. The aim of this study was to evaluate the capacity of metronidazole biotransformation through the filamentous fungus Cunninghamella elegans ATCC 9245. The monitoring of metabolite formation was performed by high-performance liquid chromatography (HPLC) coupled to ultraviolet (UV) spectrophotometry. The results of the biotransformation of metronidazole showed drug consumption in culture and the formation of four new chromatographic peaks of chemical structures not elucidated. The method showed it became linear over 10-70 μg/mL (r = 0.999953). Accuracy, precision and stability studies agree with international guidelines. Results are consistent in accordance with the principles of green chemistry as the experimental conditions had a low environmental impact, and few solvents use. ","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77839918","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRY AND LIQUID CHROMATOGRAPHY METHODS FOR DETERMINATION OF CEFPIROME IN RAW MATERIAL AND PHARMACEUTICAL DOSAGE","authors":"T. P. Oppe, Júlia Menegola, E. Schapoval","doi":"10.22456/2527-2616.93809","DOIUrl":"https://doi.org/10.22456/2527-2616.93809","url":null,"abstract":"In the present work, analytical methods, UV Spectrophotometry and Liquid Chromatography (HPLC), were developed and validated for quantification of cefpirome, a broad-spectrum fourth-generation cephalosporin, in raw material and powder for injectable preparation. The UV spectrophotometric method was performed at 271 nm, using 0.1 M hydrochloric acid as solvent. The HPLC was carried out using Techsphere ODS column and mobile phase consisted of methanol-water (30:70, v/v) with flow rate 0.8 mL/min and UV detection at 265 nm. The validation method yielded good results demonstrated statistically that the methods were linear, precise, accurate, specific and robust. A preliminary stability study of cefpirome showed that the UV Spectrophotometry and Liquid Chromatography methods were specific for the determination cefpirome in the presence of its degradation products. No statistically difference was observed between the proposed methods. The UV Spectrophotometry and Liquid Chromatography methods allow the quantitation of cefpirome in pharmaceutical dosage form and raw material and can be used for the drug analysis in routine quality control. ","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82225355","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bianca Aparecida de Marco, A. Kogawa, H. R. Salgado
{"title":"NEW, GREEN AND MINIATURIZED ANALYTICAL METHOD FOR DETERMINATION OF CEFADROXIL MONOHYDRATE IN CAPSULES","authors":"Bianca Aparecida de Marco, A. Kogawa, H. R. Salgado","doi":"10.22456/2527-2616.91086","DOIUrl":"https://doi.org/10.22456/2527-2616.91086","url":null,"abstract":"Cefadroxil, an oral antimicrobial, presents few techniques optimized for the reduction of solvents and toxic residues and/or non-use of them. So, a quantitative, new and miniaturized method for determination of cefadroxil monohydrate in capsules has been developed and validated by spectrophotometric method in the visible region according to the international guidelines. The analyzes were performed using microplates containing 96 wells, 1 % of phenolphthalein and sodium hydroxide 0.1 M as reagent at 552 nm. The method was (i) linear in the range of 15-115 µg mL-1, (ii) selective when comparing standard, sample, adjuvants and color reagent, (iii) precise with deviations below 4 %, (iv) accurate when comparing the proposed method with the HPLC method, (v) robusts by making small and deliberate modifications to the method, (vi) besides being fast, low cost, eco-friendly and generates minimal amount of waste. The method can be applied to the routine quality control of cefadroxil monohydrate in capsules and an effective and accessible alternative that contemplates the concepts of current and sustainable green analytical chemistry.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77317889","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}