Marillia Castilho Silva Toti, R. Bonfilio, M. B. de Araújo
{"title":"应用多元优化策略验证 RP-HPLC 分析方法,用于测定药品中的硫酸羟氯喹并进行强制降解研究","authors":"Marillia Castilho Silva Toti, R. Bonfilio, M. B. de Araújo","doi":"10.1556/1326.2023.01193","DOIUrl":null,"url":null,"abstract":"In this study, a multivariate optimization strategy was used to develop and validate a simple, rapid, accurate, cost-effective, and stability-indicative RP-HPLC analytical method for quantifying hydroxychloroquine sulphate (HCQ) in coated tablets. The validation conditions involved isocratic elution mode, using a mixture of buffer solution at pH 2.2 and methanol (74:26, v/v) as the mobile phase, an Agilent® reverse phase column, model Zorbax Eclipse Plus C18 (250 cm × 4.6 mm × 5 μm), a flow rate of 1.3 mL min−1, column temperature 40 °C and detection at 343 nm. The method showed linearity in the range of 4–44 μg mL−1, with a correlation coefficient (R) of 0.9998. Recovery obtained average values of between 99.71 and 100.84% and precision with average RSD values of <2%. The robustness demonstrated by assessing the effect of seven variables (pH of the mobile phase buffer; percentage of methanol; filter brand; mobile phase flow rate; wavelength; column temperature and sample agitation time), with effect values for each variable lower than the calculated value of s√2 (1.43), showed that none of these factors had a significant influence on the analytical response. The method was applied to samples of the reference medicine Plaquinol® 400 mg and similar Reuquinol 400 mg, nomenclature established by the National Health Surveillance Agency (Anvisa), law no. 978 of 10 February 1999, purchased from local pharmacies. Results showed advantages and benefits in relation to the official method and those reported in the literature. The application of the multivariate strategy, the choice of methanol, in a lower proportion in the organic phase, due to its low toxicity, economy and easier availability compared to acetonitrile, and the other organic solvents used was a promising and important alternative for the analytical method. Furthermore, the use of reversed stationary phase, common in quality control laboratories, provided an analyte retention time of 4.595 min, demonstrating good performance and speed in routine analyses.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.7000,"publicationDate":"2024-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Application of a multivariate optimization strategy to validate an RP-HPLC analytical method for determining hydroxychloroquine sulphate in pharmaceutical products and in forced degradation studies\",\"authors\":\"Marillia Castilho Silva Toti, R. Bonfilio, M. 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The robustness demonstrated by assessing the effect of seven variables (pH of the mobile phase buffer; percentage of methanol; filter brand; mobile phase flow rate; wavelength; column temperature and sample agitation time), with effect values for each variable lower than the calculated value of s√2 (1.43), showed that none of these factors had a significant influence on the analytical response. The method was applied to samples of the reference medicine Plaquinol® 400 mg and similar Reuquinol 400 mg, nomenclature established by the National Health Surveillance Agency (Anvisa), law no. 978 of 10 February 1999, purchased from local pharmacies. Results showed advantages and benefits in relation to the official method and those reported in the literature. The application of the multivariate strategy, the choice of methanol, in a lower proportion in the organic phase, due to its low toxicity, economy and easier availability compared to acetonitrile, and the other organic solvents used was a promising and important alternative for the analytical method. Furthermore, the use of reversed stationary phase, common in quality control laboratories, provided an analyte retention time of 4.595 min, demonstrating good performance and speed in routine analyses.\",\"PeriodicalId\":7130,\"journal\":{\"name\":\"Acta Chromatographica\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.7000,\"publicationDate\":\"2024-02-05\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Acta Chromatographica\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.1556/1326.2023.01193\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Acta Chromatographica","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1556/1326.2023.01193","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Application of a multivariate optimization strategy to validate an RP-HPLC analytical method for determining hydroxychloroquine sulphate in pharmaceutical products and in forced degradation studies
In this study, a multivariate optimization strategy was used to develop and validate a simple, rapid, accurate, cost-effective, and stability-indicative RP-HPLC analytical method for quantifying hydroxychloroquine sulphate (HCQ) in coated tablets. The validation conditions involved isocratic elution mode, using a mixture of buffer solution at pH 2.2 and methanol (74:26, v/v) as the mobile phase, an Agilent® reverse phase column, model Zorbax Eclipse Plus C18 (250 cm × 4.6 mm × 5 μm), a flow rate of 1.3 mL min−1, column temperature 40 °C and detection at 343 nm. The method showed linearity in the range of 4–44 μg mL−1, with a correlation coefficient (R) of 0.9998. Recovery obtained average values of between 99.71 and 100.84% and precision with average RSD values of <2%. The robustness demonstrated by assessing the effect of seven variables (pH of the mobile phase buffer; percentage of methanol; filter brand; mobile phase flow rate; wavelength; column temperature and sample agitation time), with effect values for each variable lower than the calculated value of s√2 (1.43), showed that none of these factors had a significant influence on the analytical response. The method was applied to samples of the reference medicine Plaquinol® 400 mg and similar Reuquinol 400 mg, nomenclature established by the National Health Surveillance Agency (Anvisa), law no. 978 of 10 February 1999, purchased from local pharmacies. Results showed advantages and benefits in relation to the official method and those reported in the literature. The application of the multivariate strategy, the choice of methanol, in a lower proportion in the organic phase, due to its low toxicity, economy and easier availability compared to acetonitrile, and the other organic solvents used was a promising and important alternative for the analytical method. Furthermore, the use of reversed stationary phase, common in quality control laboratories, provided an analyte retention time of 4.595 min, demonstrating good performance and speed in routine analyses.
期刊介绍:
Acta Chromatographica
Open Access
Acta Chromatographica publishes peer-reviewed scientific articles on every field of chromatography, including theory of chromatography; progress in synthesis and characterization of new stationary phases; chromatography of organic, inorganic and complex compounds; enantioseparation and chromatography of chiral compounds; applications of chromatography in biology, pharmacy, medicine, and food analysis; environmental applications of chromatography; analytical and physico-chemical aspects of sample preparation for chromatography; hyphenated and combined techniques; chemometrics and its applications in separation science.