Quantitative Analysis Of Pamabrom And Ibuprofen In Synthetic Mixture Using 1st Order Derivative Spectroscopy

Objective: The preliminary goal was to develop and validate 1st order derivative spectroscopic method for quantitative analysis of Pamabrom (PAMA) which is a xanthine diuretic and ibuprofen (IBU) which is a non-steroidal anti-inflammatory agent from its synthetic mixture. Methods: Analytical method was developed on Shimadzu double beam spectrophotometer equipped with UV probe 2.42 as software using methanol as solvent. Quantification of PAMA was carried out at zero cross over point of IBU that is 291 nm and for IBU, it was achieved at 278 nm which is zero cross over point of PAMA. Method was validated according to ICH Q2 R1 guidelines. Results: Method showed a linear response in the range of 2-12 µg/ml of PAMA and 20-120 µg/ml of IBU. Method was found to be accurate with recovery between 99.7–100.9 % for PAMA and 100.3–100.7 % for IBU. The method was found to be accurate and precise for quantitative analysis of PAMA and IBU. Conclusion: The developed method was successfully validated as per ICH Q2 R1 guidelines and was successfully applied for quantitative analysis of a synthetic mixture of PAMA and IBU.

Desenvolvimento e aplicação de método analítico para determinação de substâncias psicoativas em amostras biológicas de motociclistas empregando LC-MS/MS / Development and application of analytical method for psychoactive substances determination in biological samples of motorcyclists using LC-M/MS

Os acidentes de trânsito consistem em um grave problema de saúde pública, principalmente nos países em desenvolvimento. No Brasil, um dos recordistas mundiais nesse tipo de acidente, somente no ano de 2017 o número de mortos por essa causa foi de aproximadamente 35 mil, sendo que por volta de 12 mil eram motociclistas ou passageiros de moto. Dirigir sob efeito de substâncias psicoativas como drogas ilícitas e algumas classes de medicamentos pode aumentar significativamente o risco de ocorrências de acidentes automotivos. Pesquisas mostram que diversos fármacos psicoativos alteram a capacidade motora e cognitiva dos usuários, porém os únicos estudos brasileiros feitos com motociclistas avaliam a prevalência de uso de drogas ilícitas em usuários hospitalizados, não havendo assim trabalhos sobre o uso de outras substâncias psicoativas na população em geral de motociclistas. Visando a importância desse fato, o presente projeto avaliou a prevalência de drogas ilícitas (canabinoides, estimulantes e anfetaminas) e de fármacos psicoativos pertencentes às classes dos anti-histamínicos, relaxantes musculares, benzodiazepínicos e anorexígenos nas amostras de fluido oral de motociclistas na cidade de São Paulo. Para tal, foi desenvolvido um método analítico que utiliza a técnica de cromatografia líquida acoplada à espectrometria de massas. Além do desenvolvimento de um novo método analítico que poderá ser utilizado para o monitoramento de motoristas em geral, foram obtidos dados da prevalência do uso de drogas e medicamentos pelos motociclistas na cidade São Paulo, contribuindo assim para o desenvolvimento de medidas preventivas, políticas públicas e para o esclarecimento sobre os riscos de dirigir sob efeito de substâncias psicoativas

Traffic accidents are a serious public health problem, especially in developing countries. In Brazil, one of the world record holders in this kind of accident, in 2017 the number of death due to this cause was approximately 35 thousand, and nearly 12 thousand were motorcyclists or motorcycle passengers. Driving under the influence of psychoactive substances such as illicit drugs and some prescription drugs can significantly increase the risk of motor vehicle accidents. Researches shows that several psychoactive drugs alter the motor and cognitive capacity of users, but the few studies done in Brazil with motorcyclists evaluate the prevalence of illicit drug use in hospitalized users, thus there is no work on the use of other psychoactive substances in the general population of bikers. Considering the importance of this fact, the present project evaluated the prevalence of illicit drugs (cannabinoids, stimulants, and amphetamines) and psychoactive prescription drugs belonging to the classes of antihistamines, muscle relaxants, benzodiazepines and anorectics in motorcyclist's oral fluid samples in the city of São Paulo. Therefore, an analytical method has been developed using liquid chromatography coupled to mass spectrometry. A new analytical method was developed and validated and may be used to monitor drivers in general. Data about drugs prevalence and drug use by motorcyclists in São Paulo city were obtained contributing to the development of preventive measures, public policies and for clarification on the risks of driving under the influence of psychoactive substances

Improved RP-HPLC Method for Quantitation of Swertiamarin from Swertia Densifolia Leaves and Marketed Herbal Formulations.

Objective: Present study aims at developing and validating an improved RP-HPLC method for determination of Swertiamarin from extracts of Swertia densifolia (Griseb.) Kashyap leaves and marketed herbal formulations. Methods: Developed RP-HPLC method is validated and is used for determination of Swertiamarin from hydroalcoholic extracts of test plant material and marketed herbal formulations. The separation is carried out on C18 column. The mobile phase used is 10 mM Ammonium acetate: Acetonitrile: Formic acid in ratio 90:10:0.2% (v/v/v/). The wavelength selected is 237 nm using UV detector. Results and Discussion: A seven-point calibration curve over the concentration range of 50.00 –20000.00 ng/mL for Swertiamarin provides an optimum linear detector response (with r2>0.9970). The % R.S.D. (n = 6) for the low, middle and high quality control samples are within <6.44 and < 9.04 for inter-day and intra-day precision and accuracy respectively. Conclusion: A simple, sensitive and precise method is developed for quantitation of SWM. Method is validated as per International Conference on Harmonization (ICH) guidelines and its applicability is demonstrated by successful measurement of Swertiamarin from hydroalcoholic extracts of Swertia densifolia leaves and selected marketed herbal formulations.

Total polyphenols from syzygium cumini (L) skeels fruit extract / Polifenóis totais de Ssyzygium cumini (L) skeels extrato de frutas

A precise, accurate and low cost spectrophotometric method was developed and validated for routine determination of total polyphenols, as pyrogallic acid equivalents, from the percolated and lyophilized extract of Syzygium cumini (L.) Skeels fruits. Validation was assessed experimentally and data were rigorously treated by statistical analysis. Analytical parameters were: linearity, interval (range), precision and recovery/accuracy, limit of detection (LOD, μg mL-1) and limit of quantification (LOQ, μg mL-1). The visible spectrophotometric method presented linearity (r² = 0.9979 ± 0.0010) over the concentration range 0.25-7.5 μg mL-1 of standard pyrogallic acid, precision < 2.918171 percent, recovery/accuracy ranging from 96.228693 to 107.17701 percent, LOD = 0.21 μg mL-1 and LOQ = 0.64 μg mL-1.

Um método espectrofotométrico preciso, rigoroso e de baixo custo foi desenvolvido e validado para a determinação de polifenóis totais, utilizando-se como padrão o ácido pirogálico. O extrato dos frutos de Syzygium cumini (L.) Skeels foi preparado empregando-se o método de percolação com posterior liofilização. A validação foi executada experimentalmente e os dados foram submetidos à análise estatística. Os parâmetros analíticos considerados foram: linearidade, intervalos de precisão e de recuperação, limite de detecção (LD, μg.mL-1) e o limite de quantificação (LQ, μg.mL-1). O método espectrofotométrico apresentou linearidade (r² = 0,9979 + 0,0010) ao longo do intervalo de concentração de 0,25-7,5 μg mL-1 de ácido pirogálico, padrão de precisão menor do que 2,918171 por cento; recuperação/precisão entre 96,228693 a 107,17701 por cento, e LD = 0,21 μg-mL-1 e LOQ = 0,64 μg mL-1.