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Bacterial Inactivation Studies in Shrimp Pond Water by using Different Disinfectant Agents 使用不同消毒剂对虾池水进行细菌灭活研究
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-09-18 DOI: 10.1093/jaoacint/qsae073
Ranjit Kumar Nadella, Satyen Kumar Panda, Devananda Uchio, Pankaj Kishore, Madhu V.R, Minimol Vallamattath Ayyappan, Madhusudana Rao Badireddy, Pani Prasad Kuricheti, Ram Prakash Raman, Mukteswar Prasad Mothadaka
{"title":"Bacterial Inactivation Studies in Shrimp Pond Water by using Different Disinfectant Agents","authors":"Ranjit Kumar Nadella, Satyen Kumar Panda, Devananda Uchio, Pankaj Kishore, Madhu V.R, Minimol Vallamattath Ayyappan, Madhusudana Rao Badireddy, Pani Prasad Kuricheti, Ram Prakash Raman, Mukteswar Prasad Mothadaka","doi":"10.1093/jaoacint/qsae073","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae073","url":null,"abstract":"Background Aquaculture water plays an important role in the dissemination of antibiotic-resistant bacteria during harvest of shrimps. Mitigation of bacteria through discharge is essential to prevent dissemination downstream. Chemical disinfection of culture water is feasible compared to other methods of bacterial inactivation. Objective To study the effect of different disinfectant agent’s viz., chlorine, Fenton’s reagent, and hydrogen peroxide (H2O2) on inactivation of bacteria from shrimp pond water Methods The water samples were subjected to treatment with various concentrations of chlorine (0.0, 1.0, 2.5, 5.0 and 10.0 mg L−1), Fenton’s reagent (1:10 mM ratio of Fe2+:H2O2; 2:20, 3:30, 4:40, 5:50) and H2O2 (20, 30, 40 and 50 mM) for different time durations (5 min, 15 min, 30 min and 60 min). Results The results indicated that all the disinfecting agents inactivated both the total heterotrophic bacteria and tetracycline-resistant bacteria with increased concentrations and time. At the end of 60 min treatment with chlorination (2.5 mg Cl2 L−1), Fenton’s reagent (2 mM Fe2+ + 20 mM H2O2) and H2O2 (50 mM H2O2), the total heterotrophic bacterial count in the water samples gradually decreased by 2.35, 2.65, and 1.38 log10 CFU mL−1, and tetracycline-resistant bacteria count reduced by 1.57, 1.66, and 1.43 log10 CFU mL−1, respectively from initial bacterial load. Conclusions The study revealed that disinfection agents can be successfully employed in the inactivation of antibiotic-resistant bacteria discharged through aquaculture water. Among three disinfection agents, Fenton’s reagent has been found effective in inhibiting both heterotrophic bacteria and tetracycline-resistant bacteria from water samples. Highlights Bacterial inactivation studies were carried with Chlorination, Fenton’s reagent, and Hydrogen peroxide. The highest decrease in HPC (2.65 log) and tetracycline-resistant bacterial (1.66 log) was noticed in the water samples treated with Fenton’s reagent. The use of disinfection agents effectively mitigates antibiotic-resistant bacteria from aquaculture wastewater.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268352","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Ivermectin-based products in the context of green pharmaceutical analysis 绿色药物分析中的伊维菌素类产品
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-09-18 DOI: 10.1093/jaoacint/qsae072
Natália Sabina dos Santos Galvão, Ana Carolina Kogawa
{"title":"Ivermectin-based products in the context of green pharmaceutical analysis","authors":"Natália Sabina dos Santos Galvão, Ana Carolina Kogawa","doi":"10.1093/jaoacint/qsae072","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae072","url":null,"abstract":"Background Ivermectin (IVE), a broad-spectrum antiparasitic, is used in human and animal health. Analytical methods for evaluating IVE in pharmaceutical products are found in the literature and in official compendiums. However, the vast majority of them do not have an eco-friendly approach. Objective and Method The aim of this review is to present an overview of existing analytical methods for evaluating IVE in pharmaceutical matrices in the context of Green Analytical Chemistry (GAC) and show possibilities for increasing their greenness. Results GAC is a current alternative to promote sustainable development in laboratories and chemical-pharmaceutical industries, therefore, through its principles, such as reducing the use of aggressive solvents, it is possible to make processes more ecological. However, the vast majority of analytical methods available in the literature and official compendiums do not present an eco-friendly approach. 70% of the methods are by HPLC. Among the various pharmaceutical matrices, the most evaluated are tablets (37%). Of all the solvents used in HPLC, UPLC, HPLC-MS/MS, UV and TLC methods, the combination of methanol and acetonitrile is the most chosen, accounting for more than 50% of occurrences. Conclusions Analytical methods for evaluating IVE-based products can be leveraged within the scope of GAC, bringing sustainable work opportunities to analytical development laboratories around the world. Highlights This review shows an overview of the analytical methods present in the literature and official compendiums to evaluate pharmaceutical IVE matrices, in the context of green analytical chemistry.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268353","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Comparison of Roka Atlas® System Performance and Health Canada Reference Method for Listeria Detection from Plastic, Sealed Concrete, and Stainless Steel Surface Samples 从塑料、密封混凝土和不锈钢表面样品中检测李斯特菌的 Roka Atlas® 系统性能与加拿大卫生部参考方法的比较
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-09-14 DOI: 10.1093/jaoacint/qsae071
Fereidoun Forghani, Eni Themeli, Tam Mai, Mansour Samadpour
{"title":"Comparison of Roka Atlas® System Performance and Health Canada Reference Method for Listeria Detection from Plastic, Sealed Concrete, and Stainless Steel Surface Samples","authors":"Fereidoun Forghani, Eni Themeli, Tam Mai, Mansour Samadpour","doi":"10.1093/jaoacint/qsae071","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae071","url":null,"abstract":"Background There is a high demand in food industry and public health for rapid automated methods capable of high volume sample processing. Objective In an unpaired study Roka Atlas® System performance was compared with Health Canada reference method MFHPB-30 for Listeria spp. (LSP Roka assay) and Listeria monocytogenes (LmG2 Roka Assay) detection on plastic (PL), sealed concrete (SC), and stainless steel (SS) surfaces (45 samples each per candidate or reference method). Methods Seeking shorter enrichment time for the candidate method, R2 medium pre-enrichment for 14, 16, and 24 h at 35 °C was combined with the Roka assay. Listeria welshimeri, L. innocua, and L. monocytogenes were employed to individually inoculate each of the three surfaces, with two competing microorganisms within the 10–100 fold higher concentration range. Results False negative, false positive, sensitivity and specificity were 0, 0, 100, and 100%, respectively, for the plastic, sealed concrete, and stainless steel surfaces, regardless of inoculation level (high, low, and uninoculated) and enrichment time. Candidate method detected 10, 7 and 9 true positives, versus 10, 6 and 10 by the reference method in individually inoculated SS, PL and SC, respectively. Conclusion Probability of detection for all the three surfaces for the Roka Atlas® System was comparable to the reference method, in this unpaired study. Highlights The Roka Atlas® System detected targets after as little as 14 h enrichment. Surface type did not negatively affect assay sensitivity or specificity. The Roka Atlas® System was comparable to the reference method.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268354","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using HPLC Multi-Laboratory Validation Study, AOAC 2016.09, Final Action Status 利用 HPLC 多实验室验证研究测定原材料和成品中的芦荟素 A、芦荟素 B 和芦荟大黄素,AOAC 2016.09,最终行动状态
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-09-09 DOI: 10.1093/jaoacint/qsae070
Isaac Lee, Quanyin Gao, Wei Liu, Darshan Patel, Malissa Smith, Hong You, Tushar Patel, Karine Aylozyan, Silva Babajanian, Teddy Collins, Darryl Sullivan, Peter Chang, Gary Swanson
{"title":"Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using HPLC Multi-Laboratory Validation Study, AOAC 2016.09, Final Action Status","authors":"Isaac Lee, Quanyin Gao, Wei Liu, Darshan Patel, Malissa Smith, Hong You, Tushar Patel, Karine Aylozyan, Silva Babajanian, Teddy Collins, Darryl Sullivan, Peter Chang, Gary Swanson","doi":"10.1093/jaoacint/qsae070","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae070","url":null,"abstract":"Background A multi-laboratory validation study was performed on AOAC Official Method of Analysis (OMA) 2016.09, for final action. Eight different laboratories throughout the world participated in the study tested the same set of 6 different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria. Objective The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, limit of detection (LOD), and limit of quantitation (LOQ) by multiple laboratories to satisfy the requirement of moving the OMA 2016.09 to the final action status. Accuracy and ruggedness were already validated in earlier work of single laboratory validation (1), and it was not necessary to include these validation parameters in the multi-laboratory validation study. Method Laboratory samples containing Aloe were sent out to participating laboratories. Each lab followed AOAC 2016.09 (First Action status) to analyze contents of aloin A, aloin B, and aloe emodin using high performance liquid chromatography (HPLC) instrument. The results generated by each laboratory were collected and evaluated. Results The specificity results show that blank and matrix chromatograms do not contain major interfering peaks on the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion (ppb), 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) value of ≥ 0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The limit of detection (LOD) results show that the signal-to-noise (S/N) ratio of 10 ppb standards for all three components are about 3. The limit of quantitation (LOQ) results show that the S/N ratio of 20 ppb standards for all three components are about 10. Conclusions The validation parameters (specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ) have been successfully analyzed, and it shows that the test method is suitable for its intended use. Highlights The test method has been successfully validated by the eight different laboratories around the world (US, UK, Germany, and Canada). Each of the laboratory is managed independently by the site lab management team. This multi-lab study validated the method of Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using high performance liquid chromatography (HPLC), and the method fits for its intended purpose.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142192522","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Toxic Elements in Botanical Dietary Supplement Ingredient Reference Materials 植物膳食补充剂成分参考材料中有毒元素的测定
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-07-26 DOI: 10.1093/jaoacint/qsae064
Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise
{"title":"Determination of Toxic Elements in Botanical Dietary Supplement Ingredient Reference Materials","authors":"Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise","doi":"10.1093/jaoacint/qsae064","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae064","url":null,"abstract":"Background The National Institute of Standards and Technology (NIST) has produced over 40 botanical dietary supplement Standard Reference Materials® (SRMs) and reference materials (RMs) with values assigned for chemical markers and/or active compounds. Although environmental accumulation or inadvertent introduction of toxic elements (arsenic, cadmium, lead, and mercury) is a potential source of exposure in botanical dietary supplement products, the majority of the dietary supplement SRMs/RMs do not have values assigned for the four major toxic elements. Objective To determine As, Cd, Pb, and Hg content in the current inventory of NIST botanical dietary supplement SRMs/RMs. Methods Fifteen SRMs/RMs suites of plant part, extract, and finished products [i.e., solid oral dosage form (SODF)] were analyzed for As, Cd, Pb, and Hg using nitric acid microwave-assisted digestion followed by quantification using inductively coupled plasma—mass spectrometry. Results Results for control samples were in good agreement with certified values indicating that the analyses of 38 individual botanical SRMs/RMs were in control. Characterization of linked plant/extract SRMs/RMs derived from the same source materials demonstrated that while extraction processes can often yield extracts with lower toxic element content for Hg or As, it is also possible for mass fraction levels to remain unchanged or even increase following extraction. Conclusion The results fill significant knowledge gaps in toxic element content ranges for SRMs/RMs where no NIST assigned values existed, in particular for Hg content and for extract and SODF matrices. With comprehensive toxic element content now available, researchers can better select appropriate dietary supplement SRMs/RMs for use as controls in the analysis of dietary supplement ingredients and products. Highlights Results for As, Cd, Pb, and Hg are reported for 38 dietary supplement SRMs/RMs including 6 suites of plant, extract, and SODF and 9 pairs of plant and extract from the same batch of plant material.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141785253","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Evaluating the use of UV Absorbance for the Differentiation of Humified from Non-humified Materials 评估利用紫外线吸收率区分湿润与非湿润材料的方法
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-04-30 DOI: 10.1093/jaoacint/qsae039
Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz
{"title":"Evaluating the use of UV Absorbance for the Differentiation of Humified from Non-humified Materials","authors":"Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz","doi":"10.1093/jaoacint/qsae039","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae039","url":null,"abstract":"Background Products containing humic acids (HA) and fulvic acids (FA) have significant commercial potential, however, unknown to the consumer, some products may be mislabeled or contain adulterants. The prevalence of mislabelling and adulterants is primarily found in FA products. Using UV-Vis spectroscopy to differentiate between real and fake FA products is practical and desirable. Objective The objective of this study was to expand the data set generated using a UV-VIS based method proposed by Mayhew et al., 2023. Methods In total, thirty (30) test samples were used to generate ninety test portions (3 replicates per test sample) for analysis using the UV-Vis methodology outlined in Mayhew et al., 2023, which in this study is referred to as the UVAC (UV absorbance confirmation) method. Results None of the thirteen FA test samples investigated were determined as humified using the UVAC method. The FA samples studied comprised of two IHSS standards, five commercial FA products (CFAP) and six full FA fractions (SFA), which were isolated from six known solid humic material sources (SHMS). There was a leonardite, a humalite, and four peat sources used as the SHMS. Analysis of the neutralized extract of the SHMS found only 3/6 SHMS were determined as humified. Six HA (SHA) test samples were also generated by isolating the HA from the SHMS and only 3/6 SHA were determined as humified. Conclusion Given the high prevalence of false determinations more work is needed to improve the method so it can be used by industry or regulators. Highlights The proposed method failed to determine IHSS FA standards as humified. Although the method is practical, it needs improvement and further study before it can be used for reliable differentiation of real from fake FA or HA.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140831635","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simultaneous Determination of Fipronil, Permethrin and their Key Related Substances in a Topical Drug Product by a Single Stability Indicating High Performance Liquid Chromatography Method. 采用单一稳定性指示高效液相色谱法同时测定外用药物产品中的氟虫腈和氯菊酯及其主要相关物质
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-04-25 DOI: 10.1093/jaoacint/qsae037
Renuka P Rathnasekara, Jingzhi Tian, A. M. Rustum
{"title":"Simultaneous Determination of Fipronil, Permethrin and their Key Related Substances in a Topical Drug Product by a Single Stability Indicating High Performance Liquid Chromatography Method.","authors":"Renuka P Rathnasekara, Jingzhi Tian, A. M. Rustum","doi":"10.1093/jaoacint/qsae037","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae037","url":null,"abstract":"BACKGROUND\u0000The topical veterinary drug product containing fipronil and permethrin provides an effective repellent protection and high insecticidal efficacy for dogs.\u0000\u0000\u0000OBJECTIVE\u0000The objective of this study was to develop a stability indicating high performance liquid chromatography (HPLC) method for simultaneous detection and quantification of fipronil, permethrin, their key degradation products and butylated hydroxytoluene (BHT) in a topical drug product.\u0000\u0000\u0000METHOD\u0000The two active ingredients, their degradation products, and the antioxidant (BHT) were separated by a gradient elution on a Phenomenex Kinetex C18 column (150 × 3 mm, 2.6 µm particle size) maintained at 37 °C with H2O/acetonitrile/isopropyl alcohol/85% H3PO4 (65.5 + 32.5 + 4/0.0053, v/v/v/v) as mobile phase-A and acetonitrile (100%) as mobile phase-B. The flow rate was 0.9 mL/min and analytes were detected and quantified at 235 nm.\u0000\u0000\u0000RESULTS\u0000Specificity of the method was demonstrated by adequate separation of fipronil, permethrin, their degradation products, and BHT in the forced degraded finished product. Linearity of the method was demonstrated in the range of 0.2% to 150% of target analytical concentration of both active ingredients and 50% to 150% for BHT. Excellent recoveries of fipronil, permethrin and BHT in placebo spiked active ingredient solutions in the linearity range showed sufficient accuracy of the method. LOQ and LOD of the method were determined to be 0.2% and 0.07% of the analytical concentration. A robustness study did not identify any critical parameter that adversely effected the separation and quantification.\u0000\u0000\u0000CONCLUSIONS\u0000Here, we report the development and validation of a robust, stability indicating HPLC method for identification and assay of fipronil, permethrin, and BHT, including estimation of fipronil's and permethrin's degradation products in a topical drug product for dogs.\u0000\u0000\u0000HIGHLIGHTS\u0000The new HPLC method permits the acquisition of data for all analytes of interest for a topical finished drug product containing fipronil, permethrin, and BHT.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140657021","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Development of Two Eco-Friendly and High-Throughput Microwell Spectrophotometric Methods for Analysis of an Antibacterial Drug Tulathromycin in Pharmaceutical Bulk Form. 开发两种环保型高通量微孔分光光度法,用于分析散装抗菌药图拉霉素
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-04-23 DOI: 10.1093/jaoacint/qsae035
Ibrahim A Darwish, Nourah Z. Alzoman, M. S. Alsalhi
{"title":"Development of Two Eco-Friendly and High-Throughput Microwell Spectrophotometric Methods for Analysis of an Antibacterial Drug Tulathromycin in Pharmaceutical Bulk Form.","authors":"Ibrahim A Darwish, Nourah Z. Alzoman, M. S. Alsalhi","doi":"10.1093/jaoacint/qsae035","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae035","url":null,"abstract":"BACKGROUND\u0000Tulathromycin (TUL) is a triamilide antibacterial drug which has been approved for use in the European Union and the United States for the treatment and prevention of bovine respiratory diseases. The existing methods for determination of TUL in its pharmaceutical bulk form are very limited and suffer from major drawbacks.\u0000\u0000\u0000OBJECTIVES\u0000The aim of this study was the development of two innovative microwell spectrophotometric methods (MW-SPMs) for determination of TUL in its pharmaceutical bulk form.\u0000\u0000\u0000METHODS\u0000The formation of charge transfer complexes (CTCs) of TUL, as an electron donor, was investigated with 2,5-dihydroxy-3,6-dichlorocyclohexa-2,5-diene-1,4-dione (HCD) and 2,3-dichloro-5,6-dicyano-p-benzoquinone (CBQ), as π-electron acceptors. The CTCs were characterized by using UV-visible spectrophotometry and computational calculations. The reactions were employed for the development of two MW-SPMs with a one-step for the quantitative analysis of TUL.\u0000\u0000\u0000RESULTS\u0000The formation of CTCs was confirmed via the formation of characteristic absorption bands with maximum absorption at 520 and 460 nm for CTCs with HCD and CBQ, respectively. The stoichiometry of both CTCs was found to be 1:1, and the values of different spectroscopic and electronic constants confirmed the stability of the CTCs. The mechanisms of the reactions were postulated. The linear range of both MW-SPMs was 10-500 µg/mL. The limits of quantitation were 13.5 and 26.4 µg/mL for methods involving reactions with HCD and CBQ, respectively. Both methods were successfully applied to the quantitation of TUL in pharmaceutical bulk form with acceptable accuracy and precision. The results of eco-friendliness/greenness assessment proved that both MW-SPMs fulfill the requirements of green analytical approaches. In addition, the one-step reactions and simultaneous handling of a large number of samples with micro-volumes in the proposed methods gave them the advantage of high throughput analysis.\u0000\u0000\u0000CONCLUSIONS\u0000This study described two new MW-SPMs as valuable analytical tools for the determination of TUL.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140668138","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Integrated Multiplatform Analysis and Separation of Thirteen Flavonoids and Anthraquinones in Seven Medicinal Cassia Species. 七种药用决明中十三种黄酮类化合物和蒽醌类化合物的多平台综合分析与分离
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-04-22 DOI: 10.1093/jaoacint/qsae028
A. Girme, G. Saste, Azazahemad A. Kureshi, Shubham Jagtap, Siddhi Kamble, Saurabh D Wadye, L. Hingorani
{"title":"Integrated Multiplatform Analysis and Separation of Thirteen Flavonoids and Anthraquinones in Seven Medicinal Cassia Species.","authors":"A. Girme, G. Saste, Azazahemad A. Kureshi, Shubham Jagtap, Siddhi Kamble, Saurabh D Wadye, L. Hingorani","doi":"10.1093/jaoacint/qsae028","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae028","url":null,"abstract":"BACKGROUND\u0000Cassia (Family: Fabaceae) species are a large group of flowering plants rich in bioactive anthraquinone and flavonoids used in botanical supplements and nutraceuticals.\u0000\u0000\u0000OBJECTIVE\u0000A simple and reliable high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and validated for separating and quantifying thirteen anthraquinone and flavonoids. These compounds were further confirmed using an LC-based electrospray ionization mass spectrometry (ESI-MS/MS) method in the leaves and flowers of selected Cassia species. A simple and rapid HPTLC method was developed for chemical fingerprint analysis of all Cassia species.\u0000\u0000\u0000METHOD\u0000All thirteen compounds were chromatographically separated on a Zorbax TC18 (4.6 x 250, 5 μm particle size) analytical column, and 0.1% formic acid and acetonitrile as elution solvents at a flow rate of 0.8 mL/min with detection at 259 nm. For HPTLC fingerprinting, the mobile phase compositions of toluene, ethyl acetate, and formic acid (5.5:4.2:0.6, v/v/v) were optimized to separate and identify all compounds using silica gel 60F254 aluminum plates.\u0000\u0000\u0000RESULTS\u0000The validation data for the developed HPLC-PDA method for thirteen compounds showed good linearity (r2 > 0.99) with a sensitive LOD (0.082-1.969 mg/mL), LOQ (0.250-5.967 mg/mL), and excellent recoveries (85.22-100.32%). The quantification results were found to be precise and accurate (<5.0% and relative error), -0.77-0.44 with ESI-MS/MS confirmation in the Cassia samples. The novel HPTLC method was excellent separation for thirteen compounds, with Rf values ranging between 0.12- 0.61.\u0000\u0000\u0000CONCLUSIONS\u0000The developed HPLC-PDA method was simple, and precise and could separate and quantify anthraquinones and flavonoids along with confirmation, using a novel LC-based ESI-MS/MS. The HPTLC method was found to be simple and precise, with excellent separation capabilities for these compounds.\u0000\u0000\u0000HIGHLIGHTS\u0000This novel multiplatform approach successfully identified and quantified thirteen compounds simultaneously using an integration of data strategy in seven medicinally important Cassia species' leaves and flowers.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140677725","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Development of Analytical Quality by Design RP-HPLC Method and Its Validation for Estimation of Gefitinib from Bulk, Tablet Dosage Form and Complex Nanoformulation. 通过设计开发 RP-HPLC 分析方法及其验证,用于估算散装、片剂和复合纳米制剂中的吉非替尼。
IF 1.6 4区 农林科学
Journal of AOAC International Pub Date : 2024-04-22 DOI: 10.1093/jaoacint/qsae033
Mahesh P. More, Sagar R. Pardeshi, Rahul Tade, P. D. Meshram, Jitendra B Naik, Prashant K. Deshmukh
{"title":"Development of Analytical Quality by Design RP-HPLC Method and Its Validation for Estimation of Gefitinib from Bulk, Tablet Dosage Form and Complex Nanoformulation.","authors":"Mahesh P. More, Sagar R. Pardeshi, Rahul Tade, P. D. Meshram, Jitendra B Naik, Prashant K. Deshmukh","doi":"10.1093/jaoacint/qsae033","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae033","url":null,"abstract":"BACKGROUND\u0000Estimation of the drug and development of the method is a critical aspect of formulation development and a critical factor for analytical scientists. Gefitinib is a poorly soluble anticancer drug.\u0000\u0000\u0000OBJECTIVE\u0000The present research enlightens the topic of the development of innovative quality by design methods for the estimation of Gefitinib (GF) from bulk, pharmaceutical tablet formulation and complex nanoformulations.\u0000\u0000\u0000METHODS\u0000To simplify the estimation of poorly soluble drugs like GF, Response Surface Methodology (RSM) was adopted with effective leverages to obtain precise computation design space using the Box-Behnken Design (BBD) model. The major 3 mixed effect independent factors (Percentage of Buffer, pH of buffer and flow rate) were screened with 3 prominent dependent responses (viz., Theoretical Plate, Retention Time, and Tailing Factor) selected for optimal analysis. Furthermore, co-processed steps were employed for the estimation of the analyte from the complex formulation.\u0000\u0000\u0000RESULTS\u0000The RP-HPLC method utilizes the quality by design (QbD) approach can effectively estimate the analyte concentration of less than 4.5 min. The developed method was economically robust, and sensitive and shows a % relative standard deviation (%RSD) of less than 2% for all the selected validation parameters. The estimated design space suggests the highest desirability (R2-0.998) at 60% of buffer in the mobile phase, pH 4.25, and flow rate of 0.7 mL/min.\u0000\u0000\u0000CONCLUSION\u0000The QbD approach was used to design and develop the method by understanding the interaction between dependent and independent variables to get the optimum values. The developed method was validated successfully and can be useful for formulation scientists to estimate drug concentration and drug release profiles from complex nanoformulations.\u0000\u0000\u0000HIGHLIGHTS\u0000The analytical approach was designed and quantified using a quality-by-design approach to make the RP-HPLC method more robust and efficient for the estimation of analytes from complex nanoformulations. The method is also useful to eliminate the interfering molecule during estimation by employing co-processing steps. The developed method saves time, and cost of solvent and employs QbD as a requirement of recent regulatory concern.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140673217","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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