Pub Date : 2019-07-17DOI: 10.22456/2527-2616.91896
D. R. Nogueira-Librelotto, L. E. Scheeren, C. Rolim, L. B. Macedo, J. R. Fernandes
A stability-indicating micellar electrokinetic capillary chromatography (MEKC) method was developed and validated for the analysis of doxorubicin hydrochloride in injectable pharmaceutical dosage forms, using methotrexate as internal standard. A fused-silica capillary (50 µm i.d.; effective length, 40 cm) and a running electrolyte solution consisting of 10 mM borate buffer and 20 mM anionic surfactant SDS, at pH 9.3, were set as the best experimental conditions. Moreover, the capillary temperature was maintained at 26 ºC, while the applied voltage was +26 kV. Hydrodynamic sample injection (6 s at 50 mbar) was used, and the detection was set at 260 nm using a photodiode array detector. The method was validated for the requirements specificity, linearity, precision, accuracy, and robustness, following the International Conference on Harmonisation (ICH) guidelines. The method linearity was proven in the range of 25-125 µg/mL (r = 0.9995). Forced degradation studies were successfully conducted, evidencing the specificity and stability-indicating capability of the method. In addition, no interference of the excipients from the formulation was detected. The values of accuracy and precision were within the acceptable limits, and robustness studies were performed by a two-level full factorial design. The proposed method fulfilled all validation parameters and was shown to be suitable for quantitative analyses of doxorubicin, contributing, thus, to the establishment of new alternatives with advantages for the quality control of pharmaceutical formulations.
{"title":"DETERMINATION OF DOXORUBICIN HYDROCHLORIDE IN PHARMACEUTICA DOSAGE FORMS BY A SIMPLE STABILITY-INDICATING MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY METHOD","authors":"D. R. Nogueira-Librelotto, L. E. Scheeren, C. Rolim, L. B. Macedo, J. R. Fernandes","doi":"10.22456/2527-2616.91896","DOIUrl":"https://doi.org/10.22456/2527-2616.91896","url":null,"abstract":"A stability-indicating micellar electrokinetic capillary chromatography (MEKC) method was developed and validated for the analysis of doxorubicin hydrochloride in injectable pharmaceutical dosage forms, using methotrexate as internal standard. A fused-silica capillary (50 µm i.d.; effective length, 40 cm) and a running electrolyte solution consisting of 10 mM borate buffer and 20 mM anionic surfactant SDS, at pH 9.3, were set as the best experimental conditions. Moreover, the capillary temperature was maintained at 26 ºC, while the applied voltage was +26 kV. Hydrodynamic sample injection (6 s at 50 mbar) was used, and the detection was set at 260 nm using a photodiode array detector. The method was validated for the requirements specificity, linearity, precision, accuracy, and robustness, following the International Conference on Harmonisation (ICH) guidelines. The method linearity was proven in the range of 25-125 µg/mL (r = 0.9995). Forced degradation studies were successfully conducted, evidencing the specificity and stability-indicating capability of the method. In addition, no interference of the excipients from the formulation was detected. The values of accuracy and precision were within the acceptable limits, and robustness studies were performed by a two-level full factorial design. The proposed method fulfilled all validation parameters and was shown to be suitable for quantitative analyses of doxorubicin, contributing, thus, to the establishment of new alternatives with advantages for the quality control of pharmaceutical formulations.","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":"81937661","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 : 2018-12-16DOI: 10.22456/2527-2616.87929
Juliana Feitosa dos Santos, P. Rosa, A. I. Adams
Baclofen is a muscle relaxant used as a first option to treat spasticity and muscle spasms in patients with spinal cord injuries, which is available in Brazil as 10 mg tablets. The compendia methods employ HPLC by ion pairing that requires the use of specific reagents and column conditioning, increasing the waste generation and the cost of analysis. In this study, an isocratic, simple and stability-indicating HPLC method was validated to assay baclofen tablets. A C-18 column (Luna®, 150 x 4.6 mm, 5μm), mobile phase composed by triethylamine 10 mM pH 7.0, methanol and acetonitrile (80:15:5), flow rate 1 mL/min and detection at 220 nm was used. The baclofen retention time was 6.2 min and the method was linear in the range of 5 – 100 μg.mL-1 (r = 0.9999). Method selectivity was demonstrated by the forced degradation study and simultaneous analysis of baclofen impurity. The method showed accuracy (mean recovery 99.27%) and precision (RSD < 2%). The robustness was evaluated by factorial design, and the method was robust robust regarding the proposed variations. The developed method met the requirement of current guidelines, being indicative of stability and suitable for the determination of baclofen in tablets.
{"title":"VALIDATION OF A SIMPLE REVERSED PHASE-HPLC METHOD FOR THE DETERMINATION OF BACLOFEN IN TABLETS","authors":"Juliana Feitosa dos Santos, P. Rosa, A. I. Adams","doi":"10.22456/2527-2616.87929","DOIUrl":"https://doi.org/10.22456/2527-2616.87929","url":null,"abstract":"Baclofen is a muscle relaxant used as a first option to treat spasticity and muscle spasms in patients with spinal cord injuries, which is available in Brazil as 10 mg tablets. The compendia methods employ HPLC by ion pairing that requires the use of specific reagents and column conditioning, increasing the waste generation and the cost of analysis. In this study, an isocratic, simple and stability-indicating HPLC method was validated to assay baclofen tablets. A C-18 column (Luna®, 150 x 4.6 mm, 5μm), mobile phase composed by triethylamine 10 mM pH 7.0, methanol and acetonitrile (80:15:5), flow rate 1 mL/min and detection at 220 nm was used. The baclofen retention time was 6.2 min and the method was linear in the range of 5 – 100 μg.mL-1 (r = 0.9999). Method selectivity was demonstrated by the forced degradation study and simultaneous analysis of baclofen impurity. The method showed accuracy (mean recovery 99.27%) and precision (RSD < 2%). The robustness was evaluated by factorial design, and the method was robust robust regarding the proposed variations. The developed method met the requirement of current guidelines, being indicative of stability and suitable for the determination of baclofen in tablets.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79394853","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 : 2018-12-16DOI: 10.22456/2527-2616.90005
Aline Taís Fries, N. Olegario, S. Campanharo, V. Pereira, M. Steppe
Polymorphism is a relatively common phenomenon among pharmaceutical compounds, and one of the main aspects to be considered in the production and development of medications. The investigation of polymorphism associated with oxicams, a group belonging to the class of non-steroidal anti-inflammatory drugs (NSAIDs) has increased in recent years and, in the case of tenoxicam, the existence of four polymorphic forms is reported in the literature. The objective of this study was to characterize the presence of different polymorphic forms of tenoxicam in active pharmaceutical ingredient and oral pharmaceutical formulations, as well as to evaluate the influence on in vitro dissolution. The characterization of the three samples of pharmaceutical ingredient of tenoxicam from different suppliers by X-Ray Diffraction (XRD), Infrared (IR) and dissolution profile indicated the presence of a form III crystalline structure, without presenting significant differences between the in vitro dissolution profiles analyzed, and a Dissolution Efficiency (DE%) of 60.30%, 60.70% and 72.34%, respectively. When the four pharmaceutical specialties of tenoxicam were submitted to XRD analysis, they also presented form III crystalline structures. Despite this, the formulations presented different dissolution profiles and a DE% of 75.23%, 83.69%, 78.19% and 90.63%, respectively, without compromising their quality. However, often polymorphism affects physico-chemical properties of drugs, showing the importance of studying this phenomenon, by correlating the presence of crystalline structures to alterations in the quality of active ingredients and pharmaceutical products.
{"title":"EVALUATION OF THE PRESENCE OF POLYMORPHIC FORMS AND INFLUENCE ON THE DISSOLUTION PROFILE OF TENOXICAM IN ACTIVE PHARMACEUTICAL INGREDIENT AND FORMULATIONS","authors":"Aline Taís Fries, N. Olegario, S. Campanharo, V. Pereira, M. Steppe","doi":"10.22456/2527-2616.90005","DOIUrl":"https://doi.org/10.22456/2527-2616.90005","url":null,"abstract":"Polymorphism is a relatively common phenomenon among pharmaceutical compounds, and one of the main aspects to be considered in the production and development of medications. The investigation of polymorphism associated with oxicams, a group belonging to the class of non-steroidal anti-inflammatory drugs (NSAIDs) has increased in recent years and, in the case of tenoxicam, the existence of four polymorphic forms is reported in the literature. The objective of this study was to characterize the presence of different polymorphic forms of tenoxicam in active pharmaceutical ingredient and oral pharmaceutical formulations, as well as to evaluate the influence on in vitro dissolution. The characterization of the three samples of pharmaceutical ingredient of tenoxicam from different suppliers by X-Ray Diffraction (XRD), Infrared (IR) and dissolution profile indicated the presence of a form III crystalline structure, without presenting significant differences between the in vitro dissolution profiles analyzed, and a Dissolution Efficiency (DE%) of 60.30%, 60.70% and 72.34%, respectively. When the four pharmaceutical specialties of tenoxicam were submitted to XRD analysis, they also presented form III crystalline structures. Despite this, the formulations presented different dissolution profiles and a DE% of 75.23%, 83.69%, 78.19% and 90.63%, respectively, without compromising their quality. However, often polymorphism affects physico-chemical properties of drugs, showing the importance of studying this phenomenon, by correlating the presence of crystalline structures to alterations in the quality of active ingredients and pharmaceutical products.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72773275","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 : 2018-12-16DOI: 10.22456/2527-2616.89411
Jéssica Gonçalves Souza Lima, A. Kogawa, H. R. Salgado
A simple, rapid, economic and green analytical method was validated for the determination of secnidazole in tablets. The aim was to contribute to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. For the HPLC-UV method, the mobile phase was a mixture of purified water + 0.7 % acetic acid and ethanol (78:22, v/v), flow rate was 1.3 mL min-1 on column CN Phenomenex Luna (250 x 4.60 mm, 5 μm particle size), injection volume was 20 μL with UV detection at 318 nm and retention time of 4.26 minutes. The method was linear over the concentration range of 5-100 μg mL-1 (r = 0.9998) with limits of detection and quantitation of 0.533 e 1.615 μg mL-1, respectively. The precision of the method showed RSD less than 2 %. The accuracy determined by the average recoveries was 99.58 %. The secnidazole tablets were subjected to oxidation, acid, alkaline, neutral and photolysis degradation as stress conditions and the method was considered as indicative of stability. The method is adequate and safe to be a great alternative method in routine quality control analyzes for determination and quantification of secnidazole tablets.
{"title":"GREEN ANALYTICAL METHOD FOR QUANTIFICATION OF SECNIDAZOLE IN TABLETS BY HPLC-UV","authors":"Jéssica Gonçalves Souza Lima, A. Kogawa, H. R. Salgado","doi":"10.22456/2527-2616.89411","DOIUrl":"https://doi.org/10.22456/2527-2616.89411","url":null,"abstract":"A simple, rapid, economic and green analytical method was validated for the determination of secnidazole in tablets. The aim was to contribute to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. For the HPLC-UV method, the mobile phase was a mixture of purified water + 0.7 % acetic acid and ethanol (78:22, v/v), flow rate was 1.3 mL min-1 on column CN Phenomenex Luna (250 x 4.60 mm, 5 μm particle size), injection volume was 20 μL with UV detection at 318 nm and retention time of 4.26 minutes. The method was linear over the concentration range of 5-100 μg mL-1 (r = 0.9998) with limits of detection and quantitation of 0.533 e 1.615 μg mL-1, respectively. The precision of the method showed RSD less than 2 %. The accuracy determined by the average recoveries was 99.58 %. The secnidazole tablets were subjected to oxidation, acid, alkaline, neutral and photolysis degradation as stress conditions and the method was considered as indicative of stability. The method is adequate and safe to be a great alternative method in routine quality control analyzes for determination and quantification of secnidazole tablets.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82812889","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 : 2018-12-16DOI: 10.22456/2527-2616.88545
Jéssica Gonçalves Souza Lima, Bianca Aparecida de Marco, H. R. Salgado
Secnidazole is a medicine widely used in the treatment of bacterial and protozoal diseases. The free sale of this drug allows its easy access to the population and for this reason, the studies that involve the analysis of the quality control of this drug are extremely important to keep the results safe and reliable. Considering the great pharmacotherapeutic application of secnidazole and the great importance of developing new analytical methods that contribute to the environmen, the study was based on the development and validation of a new sustainable analytical method by Fourier-transform infrared spectroscopy (FT-IR) to identify and quantify secnidazole tablets. The method was duly validated according to the ICH guidelines, presenting precision, accuracy, selectivity, robustness and linearity in the concentration range of 0.5-1.3 mg/pellet. The application of this method in addition to being safe and reliable is highly favorable from an economic point of view since there is a significant reduction in the use of production costs as solvents and raw material, being fast and simple and can also be applied to other medicines.
{"title":"GREEN ANALYTICAL METHOD FOR QUANTIFICATION OF SECNIDAZOLE IN TABLETS BY FOURIER-TRANSFORM INFRARED SPECTROSCOPY (FTIR)","authors":"Jéssica Gonçalves Souza Lima, Bianca Aparecida de Marco, H. R. Salgado","doi":"10.22456/2527-2616.88545","DOIUrl":"https://doi.org/10.22456/2527-2616.88545","url":null,"abstract":"Secnidazole is a medicine widely used in the treatment of bacterial and protozoal diseases. The free sale of this drug allows its easy access to the population and for this reason, the studies that involve the analysis of the quality control of this drug are extremely important to keep the results safe and reliable. Considering the great pharmacotherapeutic application of secnidazole and the great importance of developing new analytical methods that contribute to the environmen, the study was based on the development and validation of a new sustainable analytical method by Fourier-transform infrared spectroscopy (FT-IR) to identify and quantify secnidazole tablets. The method was duly validated according to the ICH guidelines, presenting precision, accuracy, selectivity, robustness and linearity in the concentration range of 0.5-1.3 mg/pellet. The application of this method in addition to being safe and reliable is highly favorable from an economic point of view since there is a significant reduction in the use of production costs as solvents and raw material, being fast and simple and can also be applied to other medicines.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76001035","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 : 2018-12-16DOI: 10.22456/2527-2616.93309
Dar Dar
This policy brief outlines various options for distributing greenhouse gas emission allowances under a cap-and-trade program. Allowances represent a significant source of value and can be used to compensate firms or individuals affected by climate change policy or to raise funds for other socially desirable policy objectives. The basic allocation decision involves whether to freely allocate emission allowances, and if so, to whom, and whether to auction allowances, and if so, how to distribute the revenues. A number of recent cap-and-trade proposals begin with a combined approach that provides some allowances for free and auctions the rest, with the share of auctioned allowances rising over time. If free allocation is chosen, the basis for distribution must be determined. Options include granting allowances based on historical emissions (“grandfathering”), on levels of an output or input, or on an environmental performance “benchmark;” each has implications in terms of who benefits from the value of the allowances. If allowances are auctioned, in addition to deciding how the revenue generated by the auction will be used, policymakers will need to determine the type and frequency of the auction. Many of the same objectives can be met using either auction revenues or free allocation, including easing transition for affected firms and consumers and supporting new technologies. However, allocation decisions will sometimes entail trade-offs among the competing goals of achieving an equitable distribution of economic impacts, ensuring political feasibility, and minimizing overall program cost. Allowance allocation presents both a challenge and an opportunity: no allocation formula will satisfy everyone, yet allocation decisions can be made in ways that ease the transition to a low-carbon economy and enhance the likelihood of meaningful action on climate change. Congressional Policy Brief
{"title":"template","authors":"Dar Dar","doi":"10.22456/2527-2616.93309","DOIUrl":"https://doi.org/10.22456/2527-2616.93309","url":null,"abstract":"This policy brief outlines various options for distributing greenhouse gas emission allowances under a cap-and-trade program. Allowances represent a significant source of value and can be used to compensate firms or individuals affected by climate change policy or to raise funds for other socially desirable policy objectives. The basic allocation decision involves whether to freely allocate emission allowances, and if so, to whom, and whether to auction allowances, and if so, how to distribute the revenues. A number of recent cap-and-trade proposals begin with a combined approach that provides some allowances for free and auctions the rest, with the share of auctioned allowances rising over time. If free allocation is chosen, the basis for distribution must be determined. Options include granting allowances based on historical emissions (“grandfathering”), on levels of an output or input, or on an environmental performance “benchmark;” each has implications in terms of who benefits from the value of the allowances. If allowances are auctioned, in addition to deciding how the revenue generated by the auction will be used, policymakers will need to determine the type and frequency of the auction. Many of the same objectives can be met using either auction revenues or free allocation, including easing transition for affected firms and consumers and supporting new technologies. However, allocation decisions will sometimes entail trade-offs among the competing goals of achieving an equitable distribution of economic impacts, ensuring political feasibility, and minimizing overall program cost. Allowance allocation presents both a challenge and an opportunity: no allocation formula will satisfy everyone, yet allocation decisions can be made in ways that ease the transition to a low-carbon economy and enhance the likelihood of meaningful action on climate change. Congressional Policy Brief","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77784980","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 : 2018-12-16DOI: 10.22456/2527-2616.89412
L. Ghidini, A. Kogawa, H. R. Salgado
Doxycycline, an oral antimicrobial, does not present a sustainable analytical method described in the literature using liquid chromatography. A new and efficient method was developed and validated for the quantification of doxycycline tablets by HPLC-UV. Its aim is the contribution to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. The HPLC-UV method used a mixture of purified water + 0.5 % acetic acid and ethanol (40:60, v/v). The flow rate was 0.8 mL min-1, C18 Luna column, 20 μL of injected volumes at 275 nm. The samples were prepared in purified water and the method was linear over the concentration range of 20–200 μg mL-1 (r = 0.9997) with limits of detection and quantification of 1.08 and 3.27 μg mL-1, respectively. The precision of the method showed RSD 0.50 % (intra-assay), 2.35 % (inter-assay) and 1.13 % (between analysts). The accuracy of the method was determined by standard recovery and it was 99.85 %. The DOX tablets were subjected to oxidative, acid, basic, neutral and photolytic degradation and it showed be stability indicative. Statistical analysis provided reliable, safety and reproducible results. The method is considered linear, selective, precise, accurate, robust, indicative of stability and safe to be used in routine quality control analyzes for determination and quantification of doxycycline in tablets. The proposed method is an ecologically correct alternative for the evaluation of doxycycline tablets.
{"title":"ECO-FRIENDLY GREEN LIQUID CHROMATOGRAPHIC FOR DETERMINATION OF DOXYCYCLINE IN TABLETS AND IN THE PRESENCE OF ITS DEGRADATION PRODUCTS","authors":"L. Ghidini, A. Kogawa, H. R. Salgado","doi":"10.22456/2527-2616.89412","DOIUrl":"https://doi.org/10.22456/2527-2616.89412","url":null,"abstract":"Doxycycline, an oral antimicrobial, does not present a sustainable analytical method described in the literature using liquid chromatography. A new and efficient method was developed and validated for the quantification of doxycycline tablets by HPLC-UV. Its aim is the contribution to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. The HPLC-UV method used a mixture of purified water + 0.5 % acetic acid and ethanol (40:60, v/v). The flow rate was 0.8 mL min-1, C18 Luna column, 20 μL of injected volumes at 275 nm. The samples were prepared in purified water and the method was linear over the concentration range of 20–200 μg mL-1 (r = 0.9997) with limits of detection and quantification of 1.08 and 3.27 μg mL-1, respectively. The precision of the method showed RSD 0.50 % (intra-assay), 2.35 % (inter-assay) and 1.13 % (between analysts). The accuracy of the method was determined by standard recovery and it was 99.85 %. The DOX tablets were subjected to oxidative, acid, basic, neutral and photolytic degradation and it showed be stability indicative. Statistical analysis provided reliable, safety and reproducible results. The method is considered linear, selective, precise, accurate, robust, indicative of stability and safe to be used in routine quality control analyzes for determination and quantification of doxycycline in tablets. The proposed method is an ecologically correct alternative for the evaluation of doxycycline tablets.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82953473","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 : 2018-12-16DOI: 10.22456/2527-2616.86375
Bádila Regina Dalla Costa, C. D. Bertol, Daiane Anzilaggo, H. K. Stulzer, L. G. Rossato-Grando
A stability-indicating LC method was validated for the quantification of midazolam (MDZ) active pharmaceutical ingredient (API) and in pharmaceutical formulations. Isocratic chromatography was performed on C18 column with mobile phase containing methanol/acetonitrile/water (45:35:20 v/v/v) with 0.4% of triethylamine pH 6.5. The validation included specificity, linearity, accuracy, precision and robustness. In specificity, after acid, basic, neutral, oxidant and thermal degradation, it was found that the concentration of MDZ decreased substantially, with the appearance of peaks representatives of the degradation products, proving the stability-indicating power of the method. The response was linear in the range 50.0 – 250.0 µg.mL-1, with 11.73 µg.mL-1 and 3.87 µg.mL-1 as LOQ and LOD, respectively. Recoveries ranged between 98.68 and 100.41%. The relative standard deviation values for intra and interday precision were 1.11%, 0.82% and 1.47%, respectively. The tablets and injections containing MDZ were approved in the assay and content uniformity. The method can be adopted by pharmacopeias and for routine quality control for analysis of MDZ API, tablets and injection.
{"title":"STABILITY-INDICATING LC METHOD FOR THE QUANTIFICATION OF MIDAZOLAM ACTIVE PHARMACEUTICAL INGREDIENT AND IN PHARMACEUTICAL FORMULATIONS","authors":"Bádila Regina Dalla Costa, C. D. Bertol, Daiane Anzilaggo, H. K. Stulzer, L. G. Rossato-Grando","doi":"10.22456/2527-2616.86375","DOIUrl":"https://doi.org/10.22456/2527-2616.86375","url":null,"abstract":"A stability-indicating LC method was validated for the quantification of midazolam (MDZ) active pharmaceutical ingredient (API) and in pharmaceutical formulations. Isocratic chromatography was performed on C18 column with mobile phase containing methanol/acetonitrile/water (45:35:20 v/v/v) with 0.4% of triethylamine pH 6.5. The validation included specificity, linearity, accuracy, precision and robustness. In specificity, after acid, basic, neutral, oxidant and thermal degradation, it was found that the concentration of MDZ decreased substantially, with the appearance of peaks representatives of the degradation products, proving the stability-indicating power of the method. The response was linear in the range 50.0 – 250.0 µg.mL-1, with 11.73 µg.mL-1 and 3.87 µg.mL-1 as LOQ and LOD, respectively. Recoveries ranged between 98.68 and 100.41%. The relative standard deviation values for intra and interday precision were 1.11%, 0.82% and 1.47%, respectively. The tablets and injections containing MDZ were approved in the assay and content uniformity. The method can be adopted by pharmacopeias and for routine quality control for analysis of MDZ API, tablets and injection.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79388315","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 : 2018-12-16DOI: 10.22456/2527-2616.87344
S. S. Oliveira, F. S. Barbosa, L. Pezzi, E. Schapoval, A. Mendez
This work describes the development and validation of a microbiological method using the cylinder-plate assay for quantitative determination of imipenem in powder for injection. The aim was to obtain a low-cost and suitable methodology that can be alternative to physicochemical techniques already described, contributing for the quality control of this antibiotic. Firstly, the analytical conditions were optimized, testing the microorganism, inoculum concentration and best range of sample and standard concentrations, in a way that provides the adequate measurement of the inhibition halos. Staphylococcu s epidermidis ATCC 12228 was selected as test microorganism, as well as 2.0 % of inoculum concentration. The validation protocol followed the official guidelines, and the parameters evaluated were linearity, precision (intermediate precision and repeatability) and accuracy. All standard curves ranging 0.5-2.0 µg mL-1 showed r values higher than 0.999, and ANOVA confirmed that were no deviation from linearity (p-value < 0.05). The method also proved to be precise with RSD (relative standard deviation) values ranging 0.28-0.64 for repeatability and 2.49 for intermediate precision. It was performed three days of experiments, being three assays of eight plates a day. The drug mean content was 101.05%. Accuracy was assessed by recovery test, with standard recovery percentage of 101.70-107.90% (mean recovery = 104.86%), which was considered satisfactory. Therefore, the proposed microbiological method was considered validated and suitable for application in quantitative determination of this drug, being useful for quality control routine.
{"title":"MICROBIOLOGICAL ASSAY FOR QUANTITATIVE DETERMINATION OF IMIPENEM IN POWDER FOR INJECTION","authors":"S. S. Oliveira, F. S. Barbosa, L. Pezzi, E. Schapoval, A. Mendez","doi":"10.22456/2527-2616.87344","DOIUrl":"https://doi.org/10.22456/2527-2616.87344","url":null,"abstract":"This work describes the development and validation of a microbiological method using the cylinder-plate assay for quantitative determination of imipenem in powder for injection. The aim was to obtain a low-cost and suitable methodology that can be alternative to physicochemical techniques already described, contributing for the quality control of this antibiotic. Firstly, the analytical conditions were optimized, testing the microorganism, inoculum concentration and best range of sample and standard concentrations, in a way that provides the adequate measurement of the inhibition halos. Staphylococcu s epidermidis ATCC 12228 was selected as test microorganism, as well as 2.0 % of inoculum concentration. The validation protocol followed the official guidelines, and the parameters evaluated were linearity, precision (intermediate precision and repeatability) and accuracy. All standard curves ranging 0.5-2.0 µg mL-1 showed r values higher than 0.999, and ANOVA confirmed that were no deviation from linearity (p-value < 0.05). The method also proved to be precise with RSD (relative standard deviation) values ranging 0.28-0.64 for repeatability and 2.49 for intermediate precision. It was performed three days of experiments, being three assays of eight plates a day. The drug mean content was 101.05%. Accuracy was assessed by recovery test, with standard recovery percentage of 101.70-107.90% (mean recovery = 104.86%), which was considered satisfactory. Therefore, the proposed microbiological method was considered validated and suitable for application in quantitative determination of this drug, being useful for quality control routine.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79163662","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 : 2018-12-16DOI: 10.22456/2527-2616.87008
M. Ferreira, M. Schwanz, G. Cosenza, A. Henriques, L. Soares
Vanilla planifolia (Orchidiaceae) is a species that is renowned globally and represents the largest source of vanillin flavoring used in the food, cosmetic and pharmaceutical industries. This study was carried out to analyze by TLC and HPLC-PDA vanillin in herbal drug and tincture from V. planifolia. The herbal drug was obtained with hydroalcoholic solution under reflux; and a kinetic reaction was performed by TLC. The influences of solvent and herbal drug concentration were studied through an experimental design. The solutions (herbal drug, tincture and standard – vanillin) were prepared and analyzed in HPLC coupled with DAD detector, using wavelength of 280 nm. The total extraction of vanillin was achieved after three extraction cycles, using 1.0 g of herbal material and Ethanol 50% (v/v) as solvent. The method was linear (R2> 0.99) and demonstrated repeatability (RSD < 0.90), intermediate precision (RSD < 1.09), recovery (93.12-113.74%), as well as robustness (RSD < 4.33). The total content of vanillin found was 1.82 g% and 0.21 g% for herbal drug and tincture, respectively. A simple and optimized method for sample preparation by reflux was able to provide the exhaustive extraction of vanillin and does not compromise the reliability of the HPLC-PDA method. The chromatographic procedure was validated to separate and quantify vanillin in herbal material and tincture from pods of V. planifolia.
{"title":"ANALYSIS OF VANILLIN BY TLC AND HPLC-PDA IN HERBAL MATERIAL AND TINCTURE FROM Vanilla planifolia Jacks ex. Andrews","authors":"M. Ferreira, M. Schwanz, G. Cosenza, A. Henriques, L. Soares","doi":"10.22456/2527-2616.87008","DOIUrl":"https://doi.org/10.22456/2527-2616.87008","url":null,"abstract":"Vanilla planifolia (Orchidiaceae) is a species that is renowned globally and represents the largest source of vanillin flavoring used in the food, cosmetic and pharmaceutical industries. This study was carried out to analyze by TLC and HPLC-PDA vanillin in herbal drug and tincture from V. planifolia. The herbal drug was obtained with hydroalcoholic solution under reflux; and a kinetic reaction was performed by TLC. The influences of solvent and herbal drug concentration were studied through an experimental design. The solutions (herbal drug, tincture and standard – vanillin) were prepared and analyzed in HPLC coupled with DAD detector, using wavelength of 280 nm. The total extraction of vanillin was achieved after three extraction cycles, using 1.0 g of herbal material and Ethanol 50% (v/v) as solvent. The method was linear (R2> 0.99) and demonstrated repeatability (RSD < 0.90), intermediate precision (RSD < 1.09), recovery (93.12-113.74%), as well as robustness (RSD < 4.33). The total content of vanillin found was 1.82 g% and 0.21 g% for herbal drug and tincture, respectively. A simple and optimized method for sample preparation by reflux was able to provide the exhaustive extraction of vanillin and does not compromise the reliability of the HPLC-PDA method. The chromatographic procedure was validated to separate and quantify vanillin in herbal material and tincture from pods of V. planifolia.","PeriodicalId":11314,"journal":{"name":"Drug Analytical Research","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2018-12-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84017724","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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