This study aimed to revalidate an HPLC-based analytical methodology to determine tacrolimus within lipid-core nanocapsules and to evaluate the quality of such nanosystems. Chromatographic separation was achieved by employing a C18 column as a stationary phase and a ternary mixture of acetonitrile: water: phosphoric acid (700:299:1 v/v) as the mobile phase. The revalidated method proved to be linear in the range of 1-60 µg.mL−1 for tacrolimus (r2 >0.999). Detection and quantification limits were 45.38 ng.mL-1 and 137.51 ng.mL-1, respectively, which assures the methodology sensitivity. The method was also precise (RSD = 1.78% between samples). Besides, the methodology demonstrated accuracy and robustness. The lipid-core nanocapsules-loaded tacrolimus showed exclusively nanosized particles (±190 nm and polydispersity index of ≤v0.2), negative zeta potential (-13.67±1.16), and slightly acidic pH (5.58 ± 0.06), with a content of 98.90±2.32% and encapsulation rate of 99.23±0.32%. Tacrolimus-loaded in lipid-core nanocapsules-loaded tacrolimus showed stability for at least 30 days at room temperature and a sustained release profile compared to the drug in solution.
{"title":"Lipid core nanocapsules-loaded tacrolimus: Development and evaluation of quality parameters","authors":"Graziela Scheuer Gomes, L. Frank, Adriana Raffin Pohlmann, Silvia Stanisçuaki Guterres","doi":"10.22456/2527-2616.125229","DOIUrl":"https://doi.org/10.22456/2527-2616.125229","url":null,"abstract":"This study aimed to revalidate an HPLC-based analytical methodology to determine tacrolimus within lipid-core nanocapsules and to evaluate the quality of such nanosystems. Chromatographic separation was achieved by employing a C18 column as a stationary phase and a ternary mixture of acetonitrile: water: phosphoric acid (700:299:1 v/v) as the mobile phase. The revalidated method proved to be linear in the range of 1-60 µg.mL−1 for tacrolimus (r2 >0.999). Detection and quantification limits were 45.38 ng.mL-1 and 137.51 ng.mL-1, respectively, which assures the methodology sensitivity. The method was also precise (RSD = 1.78% between samples). Besides, the methodology demonstrated accuracy and robustness. The lipid-core nanocapsules-loaded tacrolimus showed exclusively nanosized particles (±190 nm and polydispersity index of ≤v0.2), negative zeta potential (-13.67±1.16), and slightly acidic pH (5.58 ± 0.06), with a content of 98.90±2.32% and encapsulation rate of 99.23±0.32%. Tacrolimus-loaded in lipid-core nanocapsules-loaded tacrolimus showed stability for at least 30 days at room temperature and a sustained release profile compared to the drug in solution.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2022-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83644043","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.120618
M. C. Santos, A. Henriques, A. Mendez
Cuphea genus (Lythraceae) comprises about 260 species. The dispersion of the genus occurs in two mains geographic centers: North and South America, with Brazil being the most Cuphea species-rich country, with approximately 104 identified species. Still poorly studied, the number of papers about genus has been growing considerably. However, a review of its analytical methods has not been previously performed. Therefore, this review aims to provide studies about different chromatographic methods used for the separation, elucidation, and identification of metabolites present in species of the Cuphea genus. Research in scientific databases like Scopus, PubMed, and Science Direct were managed, and all references were analyzed. This review covers the relevant literature until May 2021, totalizing 22 studies described on 12 species of Cuphea. Most methods were employed for chemical analysis, and just one of them was validated for quantification purposes. Thus, this review provides a brief overview of the different chromatographic methods used in the separation, elucidation, and identification of compounds on different species of the Cuphea genus.
{"title":"Analytical methods of phytochemicals from the Cuphea genus - A review","authors":"M. C. Santos, A. Henriques, A. Mendez","doi":"10.22456/2527-2616.120618","DOIUrl":"https://doi.org/10.22456/2527-2616.120618","url":null,"abstract":"Cuphea genus (Lythraceae) comprises about 260 species. The dispersion of the genus occurs in two mains geographic centers: North and South America, with Brazil being the most Cuphea species-rich country, with approximately 104 identified species. Still poorly studied, the number of papers about genus has been growing considerably. However, a review of its analytical methods has not been previously performed. Therefore, this review aims to provide studies about different chromatographic methods used for the separation, elucidation, and identification of metabolites present in species of the Cuphea genus. Research in scientific databases like Scopus, PubMed, and Science Direct were managed, and all references were analyzed. This review covers the relevant literature until May 2021, totalizing 22 studies described on 12 species of Cuphea. Most methods were employed for chemical analysis, and just one of them was validated for quantification purposes. Thus, this review provides a brief overview of the different chromatographic methods used in the separation, elucidation, and identification of compounds on different species of the Cuphea genus.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79287358","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.118887
F. Roveri, A. F. Pego, Sarah Eller, T. Oliveira, M. Yonamine
Hair analysis is thoroughly used in forensic toxicology although there are still some points of concern such as lack of reference material, whether for internal quality controls (IQC) or even for analytical validation process verification. Nonetheless spiked samples are still widely used, mainly for method development, it is not possible to evaluate its actual reproducibility and accuracy. As an alternative, IQC could be produced artificially by the laboratories themselves. The aim of this work was the evaluation of the phenomenon of artificial incorporation of drugs into hair to produce internal quality controls. These controls have been prepared according to the recommendations from the National Institute of Standards and Technology. For the amphetamine group, amphetamine and MDMA, showed different incorporation rates, of 0.17 up to 0.5% for amphetamine and 0.10 up to 0.4% for MDMA. As for cocaine, the incorporation rate was progressive over the course of days, ranging from 0.15 to 0.75%. The highest incorporation was found for diazepam, from 0.57%. to 3.75%. Lower rates were obtained for morphine, ranging from 0.08 to 0.25%, given that the incorporation rate of 0.25% has been reached on the ninth day. Some factors such as incubation time, agitation process and sample washing probably influenced the way analytes incorporate into the matrix including the effects of homogenization of the samples. Overall, knowing the incorporation profile of each analyte it is possible to produce IQC, with different concentrations. Thus, laboratories will have the fortified samples as a better tool for evaluating their own methodology.
{"title":"Evaluation of artificial drug incorporation into hair for the production of quality control samples","authors":"F. Roveri, A. F. Pego, Sarah Eller, T. Oliveira, M. Yonamine","doi":"10.22456/2527-2616.118887","DOIUrl":"https://doi.org/10.22456/2527-2616.118887","url":null,"abstract":"Hair analysis is thoroughly used in forensic toxicology although there are still some points of concern such as lack of reference material, whether for internal quality controls (IQC) or even for analytical validation process verification. Nonetheless spiked samples are still widely used, mainly for method development, it is not possible to evaluate its actual reproducibility and accuracy. As an alternative, IQC could be produced artificially by the laboratories themselves. The aim of this work was the evaluation of the phenomenon of artificial incorporation of drugs into hair to produce internal quality controls. These controls have been prepared according to the recommendations from the National Institute of Standards and Technology. For the amphetamine group, amphetamine and MDMA, showed different incorporation rates, of 0.17 up to 0.5% for amphetamine and 0.10 up to 0.4% for MDMA. As for cocaine, the incorporation rate was progressive over the course of days, ranging from 0.15 to 0.75%. The highest incorporation was found for diazepam, from 0.57%. to 3.75%. Lower rates were obtained for morphine, ranging from 0.08 to 0.25%, given that the incorporation rate of 0.25% has been reached on the ninth day. Some factors such as incubation time, agitation process and sample washing probably influenced the way analytes incorporate into the matrix including the effects of homogenization of the samples. Overall, knowing the incorporation profile of each analyte it is possible to produce IQC, with different concentrations. Thus, laboratories will have the fortified samples as a better tool for evaluating their own methodology.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87092143","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.112077
J. W. Manoel, Gabriele Bordignon Primieri, N. Volpato, M. Steppe
The present study proposes a validated dissolution method for empagliflozin (EMPA) in film coated tablets. A gradual in vitro dissolution profile for this formulation was obtained using 900 mL of hydrochloric acid 0.01 M at 37 °C ± 0.5 °C as dissolution medium and USP apparatus 2 (paddle) at 50 rpm. The dissolved percentage of EMPA was quantified by ultraviolet spectrophotometric method to obtain cost technique and produce little residual solvents. Validation parameter for dissolution methodology such as the specificity, linearity, accuracy and precision were evaluated according to the international guidelines, giving results within the acceptable range. The method is linear in the range of 1 - 40 µg/mL, precise, with RSD value less than 2.62%, accurate (mean recovery 106.97%) and robust. Therefore, since no official method has been described, the proposed dissolution conditions represent a relevant contribution to evaluate the dissolution profile of coated tablet containing 25 mg of EMPA.
本研究提出了一种有效的恩帕列净(EMPA)在薄膜包衣片中溶出度测定方法。使用900 mL盐酸0.01 M, 37°C±0.5°C作为溶出介质，USP仪器2(桨)在50 rpm转速下获得该制剂的体外逐渐溶出曲线。采用紫外分光光度法测定了EMPA的溶解率，获得了成本低、溶剂残留少的方法。根据国际指南对溶出度方法学的验证参数，如特异性、线性度、准确度和精密度进行了评估，结果在可接受范围内。该方法在1 ~ 40µg/mL范围内呈线性，精密度高，RSD值小于2.62%，准确度(平均回收率为106.97%)，鲁棒性好。因此，由于没有正式的方法描述，所提出的溶出条件代表了评估含25 mg EMPA包衣片溶出谱的相关贡献。
{"title":"Development and validation of a dissolution test for empagliflozin in film-coated tablets","authors":"J. W. Manoel, Gabriele Bordignon Primieri, N. Volpato, M. Steppe","doi":"10.22456/2527-2616.112077","DOIUrl":"https://doi.org/10.22456/2527-2616.112077","url":null,"abstract":"The present study proposes a validated dissolution method for empagliflozin (EMPA) in film coated tablets. A gradual in vitro dissolution profile for this formulation was obtained using 900 mL of hydrochloric acid 0.01 M at 37 °C ± 0.5 °C as dissolution medium and USP apparatus 2 (paddle) at 50 rpm. The dissolved percentage of EMPA was quantified by ultraviolet spectrophotometric method to obtain cost technique and produce little residual solvents. Validation parameter for dissolution methodology such as the specificity, linearity, accuracy and precision were evaluated according to the international guidelines, giving results within the acceptable range. The method is linear in the range of 1 - 40 µg/mL, precise, with RSD value less than 2.62%, accurate (mean recovery 106.97%) and robust. Therefore, since no official method has been described, the proposed dissolution conditions represent a relevant contribution to evaluate the dissolution profile of coated tablet containing 25 mg of EMPA.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83841185","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.117905
Danielle Evangelista Rabelo De Souza, Nicoly Kaliny Magela Gomes, G. A. Pianetti, B. G. Pereira, C. Fernandes
Lamivudine (3TC) and tenofovir disoproxil fumarate (TDF) are antiretroviral drugs widely used for AIDS treatment. Since safety, efficacy and quality are essential for drug products, stability studies must be performed. Therefore, degradation studies must be carried out to evaluate the degradation products formed. The active pharmaceutical ingredients 3TC and TDF, as well as the tablets containing the combination of these drugs were subjected to a comprehensive forced degradation. 3TC, TDF and the degradation products were analyzed by a stability-indicating ultra-high performance liquid chromatography (UHPLC) method developed and validated. A C8 (100 x 2.0 mm, 2.2 μm) column and a mobile phase composed of 0.1 M ammonium acetate buffer pH 4.0, acetonitrile and methanol in gradient elution, at 0.5 mL/min, were used. The injection volume was 4 μL and detection was at 260 nm. The method was selective, precise, accurate and linear in the range 0.1-0.6 mg mL-1 for the two drugs. 3TC was degraded in acidic, alkaline and oxidative environment and in the presence of metal ions. Two degradation products were observed. TDF was degraded in the same conditions than those 3TC was labile. In addition, TDF was degraded in neutral condition. Again, two degradation products were formed. Chemical structures were proposed for the degradation products using UHPLC-QTOF/MS. The stability-indicating method developed showed to be useful in stability studies and in the quality control of fixed-dose combination tablets containing 3TC and TDF.
拉米夫定(3TC)和富马酸替诺福韦二吡酯(TDF)是广泛用于艾滋病治疗的抗逆转录病毒药物。由于安全性、有效性和质量对药品至关重要，因此必须进行稳定性研究。因此，必须进行降解研究，对形成的降解产物进行评价。对活性药物成分3TC和TDF以及含这两种药物组合的片剂进行全面强制降解。采用稳定性指示的超高高效液相色谱(UHPLC)方法对3TC、TDF及其降解产物进行分析。色谱柱为C8 (100 × 2.0 mm, 2.2 μm)，流动相为0.1 M pH 4.0的醋酸铵缓冲液，乙腈和甲醇，梯度洗脱，流速为0.5 mL/min。注射量为4 μL，检测波长为260 nm。该方法在0.1 ~ 0.6 mg mL-1范围内选择性好、精密度高、准确度高、线性良好。3TC在酸性、碱性和氧化环境以及金属离子存在下均可降解。观察到两种降解产物。在相同条件下，TDF降解率高于3TC。此外，TDF在中性条件下被降解。同样，形成了两种降解产物。利用UHPLC-QTOF/MS分析了降解产物的化学结构。所建立的稳定性指示方法可用于3TC和TDF固定剂量联合片剂的稳定性研究和质量控制。
{"title":"Rapid stability-indicating UHPLC method for determination of lamivudine and tenofovir disoproxil fumarate in fixed-dose combination tablets","authors":"Danielle Evangelista Rabelo De Souza, Nicoly Kaliny Magela Gomes, G. A. Pianetti, B. G. Pereira, C. Fernandes","doi":"10.22456/2527-2616.117905","DOIUrl":"https://doi.org/10.22456/2527-2616.117905","url":null,"abstract":"Lamivudine (3TC) and tenofovir disoproxil fumarate (TDF) are antiretroviral drugs widely used for AIDS treatment. Since safety, efficacy and quality are essential for drug products, stability studies must be performed. Therefore, degradation studies must be carried out to evaluate the degradation products formed. The active pharmaceutical ingredients 3TC and TDF, as well as the tablets containing the combination of these drugs were subjected to a comprehensive forced degradation. 3TC, TDF and the degradation products were analyzed by a stability-indicating ultra-high performance liquid chromatography (UHPLC) method developed and validated. A C8 (100 x 2.0 mm, 2.2 μm) column and a mobile phase composed of 0.1 M ammonium acetate buffer pH 4.0, acetonitrile and methanol in gradient elution, at 0.5 mL/min, were used. The injection volume was 4 μL and detection was at 260 nm. The method was selective, precise, accurate and linear in the range 0.1-0.6 mg mL-1 for the two drugs. 3TC was degraded in acidic, alkaline and oxidative environment and in the presence of metal ions. Two degradation products were observed. TDF was degraded in the same conditions than those 3TC was labile. In addition, TDF was degraded in neutral condition. Again, two degradation products were formed. Chemical structures were proposed for the degradation products using UHPLC-QTOF/MS. The stability-indicating method developed showed to be useful in stability studies and in the quality control of fixed-dose combination tablets containing 3TC and TDF.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88419051","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.118365
Lionel Salem Aza-Gnandji, L. Bueno, T. P. Oppe, E. Schapoval
The objective of the study was to validate an analytical method for the quantification of ciprofloxacin in ophthalmic ointment by high performance liquid chromatography. The chromatographic separation of ciprofloxacin hydrochloride was achieved on a Thermo hypersil Gold C18 column using UV detection at 278 nm. The optimized mobile phase consisted of a mixture of 0.025 M phosphoric acid with a pH previously adjusted with triethylamine to 3.0 and acetonitrile (85:15, v / v). The validation method yielded good results demonstrated statistically that the method was linear, precise, accurate, specific and robust. No interference from any components of the pharmaceutical dosage forms was observed.
{"title":"LC method for quantitative determination of Ciprofloxacin in ophthalmic ointment","authors":"Lionel Salem Aza-Gnandji, L. Bueno, T. P. Oppe, E. Schapoval","doi":"10.22456/2527-2616.118365","DOIUrl":"https://doi.org/10.22456/2527-2616.118365","url":null,"abstract":"The objective of the study was to validate an analytical method for the quantification of ciprofloxacin in ophthalmic ointment by high performance liquid chromatography. The chromatographic separation of ciprofloxacin hydrochloride was achieved on a Thermo hypersil Gold C18 column using UV detection at 278 nm. The optimized mobile phase consisted of a mixture of 0.025 M phosphoric acid with a pH previously adjusted with triethylamine to 3.0 and acetonitrile (85:15, v / v). The validation method yielded good results demonstrated statistically that the method was linear, precise, accurate, specific and robust. No interference from any components of the pharmaceutical dosage forms was observed. ","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77977380","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.117544
Silvia Cristina Fagundes, L. G. Rossato-Grando, Camila Favretto Souza, Oberdan Fiorentin, C. M. Mistura, C. Bertol
Lead is a metal with recognized toxicity and it is known that it may be a contaminant in lipsticks. In Brazil, the Health Regulatory Agency (ANVISA) determines that the maximum limit allowed for the presence of lead in lipsticks is 20 ppm. Children are more vulnerable to lead toxicity. The objective of this study was to evaluate the presence of lead in infant lipsticks. Nineteen samples from four different brands sold in Brazil were evaluated. After sample extraction, analyses were performed by graphite furnace atomic absorption spectrometry. Lead was not detected in any of the tested lipsticks. Considering the presence of lead in adult makeup, the present study reinforces the need to use products intended for children considering kids are more vulnerable to lead toxic effects.
{"title":"Lead evaluation in children's lipsticks through atomic absorption spectrometry","authors":"Silvia Cristina Fagundes, L. G. Rossato-Grando, Camila Favretto Souza, Oberdan Fiorentin, C. M. Mistura, C. Bertol","doi":"10.22456/2527-2616.117544","DOIUrl":"https://doi.org/10.22456/2527-2616.117544","url":null,"abstract":"Lead is a metal with recognized toxicity and it is known that it may be a contaminant in lipsticks. In Brazil, the Health Regulatory Agency (ANVISA) determines that the maximum limit allowed for the presence of lead in lipsticks is 20 ppm. Children are more vulnerable to lead toxicity. The objective of this study was to evaluate the presence of lead in infant lipsticks. Nineteen samples from four different brands sold in Brazil were evaluated. After sample extraction, analyses were performed by graphite furnace atomic absorption spectrometry. Lead was not detected in any of the tested lipsticks. Considering the presence of lead in adult makeup, the present study reinforces the need to use products intended for children considering kids are more vulnerable to lead toxic effects.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83388239","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}
Pub Date : 2021-12-15DOI: 10.22456/2527-2616.120343
Idamir José Mascarello Junior, R. Sponchiado, Leticia Malgarin Cordenonsi, Tércio Oppe Oppe, E. E. S. Shapoval
The present study reports the development and validation of a microbiological assay. To assess this methodology, the method was developed and validated for the quantification of CEF by high performance liquid chromatography (HPLC). The validation of the microbial assay by diffusion method in 3x3 cylinder agar presented showed satisfactory results as to specificity, linearity in the range of 2.0 - 8.0 μg.mL-1, precision (109.42 %), accuracy (102.3 %), and robustness. The development and validation of the method by HPLC were evaluated according to specificity, linearity, precision, accuracy and robustness. A high performance liquid chromatography from Shimadzu with Agilent® C18 column, mobile phase (water with triethylamine 1.0 % pH 5.0: acetonitrile 87:13 v/v was used in the chromatographic method. The validated microbiological and chromatographic methods were compared statistically and there was no significant difference between them when compared by Student's t-test. In the preliminary stability study, it was found stable in acid hydrolysis (0.1M) and UVA light in the period evaluated, and unstable against thermal degradation (40 and 60 °C), oxidative with hydrogen peroxide, basic in NaOH (0.1 M and 0.01M) and UVC light. Samples exposed to UVC light and thermal degradation at 60°C showed degradation kinetics following zero order and second order, respectively. The cytotoxicity assay showed no difference between the normal condition and the sample submitted to forced degradation, suggesting that the possible degradation products formed did not change the result. The methods developed did not present a significant difference, therefore, they are interchangeable, and so can be used for routine quality control analysis.
{"title":"Ceftaroline fosamil: development a rapid HPLC method indicating stability and bioassay for determination in pharmaceutical formulation, stability and cytotoxicity studies","authors":"Idamir José Mascarello Junior, R. Sponchiado, Leticia Malgarin Cordenonsi, Tércio Oppe Oppe, E. E. S. Shapoval","doi":"10.22456/2527-2616.120343","DOIUrl":"https://doi.org/10.22456/2527-2616.120343","url":null,"abstract":"The present study reports the development and validation of a microbiological assay. To assess this methodology, the method was developed and validated for the quantification of CEF by high performance liquid chromatography (HPLC). The validation of the microbial assay by diffusion method in 3x3 cylinder agar presented showed satisfactory results as to specificity, linearity in the range of 2.0 - 8.0 μg.mL-1, precision (109.42 %), accuracy (102.3 %), and robustness. The development and validation of the method by HPLC were evaluated according to specificity, linearity, precision, accuracy and robustness. A high performance liquid chromatography from Shimadzu with Agilent® C18 column, mobile phase (water with triethylamine 1.0 % pH 5.0: acetonitrile 87:13 v/v was used in the chromatographic method. The validated microbiological and chromatographic methods were compared statistically and there was no significant difference between them when compared by Student's t-test. In the preliminary stability study, it was found stable in acid hydrolysis (0.1M) and UVA light in the period evaluated, and unstable against thermal degradation (40 and 60 °C), oxidative with hydrogen peroxide, basic in NaOH (0.1 M and 0.01M) and UVC light. Samples exposed to UVC light and thermal degradation at 60°C showed degradation kinetics following zero order and second order, respectively. The cytotoxicity assay showed no difference between the normal condition and the sample submitted to forced degradation, suggesting that the possible degradation products formed did not change the result. The methods developed did not present a significant difference, therefore, they are interchangeable, and so can be used for routine quality control analysis.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2021-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76928460","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}
Pub Date : 2021-06-30DOI: 10.22456/2527-2616.113283
Suelen Da Silva Reis, Valdemir Da Silva Quintanilha Junior, Gabriella Da Silva Boto, Thalita Martins Da Silva, Elizabeth Valverde Macedo, C. A. F. Peregrino, S. Mourão, Emeli Moura De Araújo
Campus compounding pharmacies play an important role in public health. Herpes simplex is one of the most common viral diseases in humans, which generates a great demand for acyclovir capsules in compounding pharmacy. It is well known that the formulation's components influence the effectiveness of the drug. The objective of this study is to show the applicability of Box-Behnken design in optimization of a compounded formulation and to evaluate the effect of excipients on dissolution and drug content in acyclovir 200 mg capsules produced at UFF´s University Pharmacy (FAU). The formulations were prepared and evaluated for average weight test, uniformity of dosage units and in vitro dissolution, while meeting pharmacopoeial specifications. A statistical analysis showed that sodium starch glycolate, Aerosil®, influences drug content and dissolution results. Magnesium stearate shows no influence on the dissolution at different concentrations but influences the assay results. A numerical optimization was applied to adjust the formulation variables based on the foresaid responses, accomplishing the best formulation that will be prepared and dispensed at FAU upon medical prescription.
{"title":"Use of Box–Behnken design for optimization of compounded medication: acyclovir capsules report","authors":"Suelen Da Silva Reis, Valdemir Da Silva Quintanilha Junior, Gabriella Da Silva Boto, Thalita Martins Da Silva, Elizabeth Valverde Macedo, C. A. F. Peregrino, S. Mourão, Emeli Moura De Araújo","doi":"10.22456/2527-2616.113283","DOIUrl":"https://doi.org/10.22456/2527-2616.113283","url":null,"abstract":"Campus compounding pharmacies play an important role in public health. Herpes simplex is one of the most common viral diseases in humans, which generates a great demand for acyclovir capsules in compounding pharmacy. It is well known that the formulation's components influence the effectiveness of the drug. The objective of this study is to show the applicability of Box-Behnken design in optimization of a compounded formulation and to evaluate the effect of excipients on dissolution and drug content in acyclovir 200 mg capsules produced at UFF´s University Pharmacy (FAU). The formulations were prepared and evaluated for average weight test, uniformity of dosage units and in vitro dissolution, while meeting pharmacopoeial specifications. A statistical analysis showed that sodium starch glycolate, Aerosil®, influences drug content and dissolution results. Magnesium stearate shows no influence on the dissolution at different concentrations but influences the assay results. A numerical optimization was applied to adjust the formulation variables based on the foresaid responses, accomplishing the best formulation that will be prepared and dispensed at FAU upon medical prescription.","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":"83226477","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}
Pub Date : 2021-06-30DOI: 10.22456/2527-2616.113058
S. Ashour
A new and direct colorimetric method has been established for the determination of catecholamine (methyldopa, MD) in both pure form and in pharmaceutical formulations. The method is based on the oxidative coupling reaction of MD with 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) and potassium ferricyanide at pH 10.4 in aqueous medium to form an orange product that has a maximum absorption at 460 nm. Beer's law plot showed good correlation in the concentration range of 1.0−56.0 µg mL-1, with detection limit of 0.31 µg mL-1. Molar absorptivity for the above method was found to be 6.56×103 L mol-1 cm-1. All the measurements were carried out at 25 ± 1.0 °C, the formation constant (logKf) value of colored species is 9.48 and the standard free energy (DG‡) is − 54.09 KJ mol-1. This method was applied successfully to determination of MD in tablets and the results were compared with the USP method. Common excipients used as additives in tablets do not interfere in the proposed method. The method is accurate, precise and highly reproducible, while being simple, cheap and less time consuming and hence can be suitably applied for routine analysis of MD in bulk and dosage forms.
{"title":"A novel sensitive colorimetric determination of catecholamine drug in dosage form via oxidative coupling reaction with MBTH and potassium ferricyanide","authors":"S. Ashour","doi":"10.22456/2527-2616.113058","DOIUrl":"https://doi.org/10.22456/2527-2616.113058","url":null,"abstract":"A new and direct colorimetric method has been established for the determination of catecholamine (methyldopa, MD) in both pure form and in pharmaceutical formulations. The method is based on the oxidative coupling reaction of MD with 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) and potassium ferricyanide at pH 10.4 in aqueous medium to form an orange product that has a maximum absorption at 460 nm. Beer's law plot showed good correlation in the concentration range of 1.0−56.0 µg mL-1, with detection limit of 0.31 µg mL-1. Molar absorptivity for the above method was found to be 6.56×103 L mol-1 cm-1. All the measurements were carried out at 25 ± 1.0 °C, the formation constant (logKf) value of colored species is 9.48 and the standard free energy (DG‡) is − 54.09 KJ mol-1. This method was applied successfully to determination of MD in tablets and the results were compared with the USP method. Common excipients used as additives in tablets do not interfere in the proposed method. The method is accurate, precise and highly reproducible, while being simple, cheap and less time consuming and hence can be suitably applied for routine analysis of MD in bulk and dosage forms.","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":"79605040","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}
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