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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 Q3 CHEMISTRY, ANALYTICAL 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
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.
背景 水产养殖用水在对虾收获过程中抗生素耐药细菌的传播中起着重要作用。通过排放减少细菌对防止向下游传播至关重要。与其他细菌灭活方法相比,对养殖水进行化学消毒是可行的。目标 研究不同消毒剂的效果,即氯气、Fenton's 反应、方法 将水样用不同浓度的氯(0.0、1.0、2.5、5.0 和 10.0 mg L-1)、芬顿试剂(Fe2+:H2O2 的比例为 1:10 mM;2:20、3:30、4:40、5:50)和 H2O2(20、30、40 和 50 mM)处理不同时间(5 分钟、15 分钟、30 分钟和 60 分钟)。结果 结果表明,随着浓度和时间的增加,所有消毒剂都能灭活全部异养菌和四环素耐药菌。在使用氯化(2.5 mg Cl2 L-1)、芬顿试剂(2 mM Fe2+ + 20 mM H2O2)和 H2O2(50 mM H2O2)处理 60 分钟后,水样中的总异养细菌数分别比初始细菌数逐渐减少了 2.35、2.65 和 1.38 log10 CFU mL-1,耐四环素细菌数分别减少了 1.57、1.66 和 1.43 log10 CFU mL-1。结论 研究表明,消毒剂可成功用于灭活养殖水体中排出的抗生素耐药菌。在三种消毒剂中,芬顿试剂能有效抑制水样中的异养菌和耐四环素细菌。要点 使用氯化、芬顿试剂和过氧化氢进行了细菌灭活研究。在使用芬顿试剂处理的水样中,HPC(2.65 log)和耐四环素细菌(1.66 log)的降幅最大。使用消毒剂可有效减少水产养殖废水中的抗生素耐药菌。
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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 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-18 DOI: 10.1093/jaoacint/qsae072
Natália Sabina dos Santos Galvão, Ana Carolina Kogawa
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.
背景 伊维菌素(IVE)是一种广谱抗寄生虫药物,用于人类和动物健康。评估药品中伊维菌素含量的分析方法见诸于文献和官方药典。然而,其中绝大多数都没有采用生态友好型方法。目的和方法 本综述旨在概述在绿色分析化学(GAC)背景下评估药物基质中 IVE 的现有分析方法,并说明提高其绿色性的可能性。结果 绿色分析化学(GAC)是目前促进实验室和化学制药行业可持续发展的一种替代方法,因此,通过其原则(如减少侵蚀性溶剂的使用),有可能使流程更加生态化。然而,文献和官方简编中的绝大多数分析方法都没有采用生态友好型方法。其中 70% 的方法采用的是高效液相色谱法。在各种药物基质中,评估最多的是片剂(37%)。在 HPLC、UPLC、HPLC-MS/MS、UV 和 TLC 方法中使用的所有溶剂中,甲醇和乙腈的组合是最常用的,占 50%以上。结论 评估基于 IVE 的产品的分析方法可在 GAC 范围内加以利用,为世界各地的分析开发实验室带来可持续的工作机会。亮点 本综述概述了在绿色分析化学背景下,文献和官方汇编中用于评估药物 IVE 基质的分析方法。
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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 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-14 DOI: 10.1093/jaoacint/qsae071
Fereidoun Forghani, Eni Themeli, Tam Mai, Mansour Samadpour
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.
背景 食品工业和公共卫生领域对能够进行大量样品处理的快速自动方法有很高的需求。目的 在一项非配对研究中,比较了 Roka Atlas® 系统与加拿大卫生部参考方法 MFHPB-30 在塑料 (PL)、密封混凝土 (SC) 和不锈钢 (SS) 表面(每种候选方法或参考方法各 45 个样品)上检测李斯特菌属 (LSP Roka 检测法) 和单核细胞增生李斯特菌 (LmG2 Roka 检测法) 的性能。方法 为了缩短候选方法的富集时间,R2 培养基在 35 °C、14、16 和 24 小时的预富集与罗卡检测相结合。采用韦氏李斯特菌、无毒李斯特菌和单核细胞增生李斯特菌分别接种于三个表面,两个竞争微生物的浓度范围在 10-100 倍以上。结果 无论接种水平(高、低和未接种)和富集时间如何,塑料、密封混凝土和不锈钢表面的假阴性、假阳性、灵敏度和特异性分别为 0、0、100 和 100%。在单独接种的 SS、PL 和 SC 中,候选方法分别检测出 10、7 和 9 个真阳性,而参考方法分别检测出 10、6 和 10 个真阳性。结论 在这项非配对研究中,Roka Atlas® 系统对所有三种表面的检测概率与参考方法相当。亮点 Roka Atlas® 系统只需经过 14 小时的富集就能检测到目标物。表面类型不会对检测灵敏度或特异性产生负面影响。Roka Atlas® 系统与参比方法具有可比性。
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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 Q3 CHEMISTRY, ANALYTICAL 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
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.
背景 对 AOAC 官方分析方法 (OMA) 2016.09 进行了一项多实验室验证研究,以便最终采取行动。全球有 8 家不同的实验室参与了这项研究,对同一套 6 种不同的原材料(商业)和配方产品(商业)实验室样品进行了测试,所有实验室都成功得出了符合验收标准的结果。目标 该研究旨在评估多个实验室的特异性、精密度(变异)、线性/范围、系统适用性、检测限 (LOD) 和定量限 (LOQ),以满足将 OMA 2016.09 移至最终行动状态的要求。准确度和耐用性已在早期的单实验室验证工作中得到验证 (1),因此没有必要将这些验证参数纳入多实验室验证研究中。方法 实验室含有芦荟的样品被发送到参与实验室。各实验室按照 AOAC 2016.09(首次行动状态)的要求,使用高效液相色谱(HPLC)仪器分析芦荟素 A、芦荟素 B 和芦荟大黄素的含量。收集并评估了各实验室得出的结果。结果 特异性结果表明,空白色谱图和基质色谱图在芦荟苷 A、芦荟苷 B 和芦荟大黄素的保留时间上不包含主要干扰峰。重复制备的样品的精密度(变异)结果相差不超过 0.05 百万分之一(ppm)。六种标准品(10ppb、20ppb、40ppb、80ppb、160ppb 和 500ppb)的线性/范围结果的相关系数(R)≥ 0.999。系统适用性结果符合仪器有效性的验收标准。检测限(LOD)结果表明,10 ppb 标准品检测三种成分的信噪比(S/N)约为 3;定量限(LOQ)结果表明,20 ppb 标准品检测三种成分的信噪比(S/N)约为 10。结论 成功分析了验证参数(特异性、精密度(变异)、线性/范围、系统适用性、LOD 和 LOQ),表明该测试方法适合其预期用途。亮点 该测试方法已成功通过全球八个不同实验室(美国、英国、德国和加拿大)的验证。每个实验室都由现场实验室管理团队独立管理。这项多实验室研究验证了使用高效液相色谱法(HPLC)测定原材料和成品中芦荟素 A、芦荟素 B 和芦荟大黄素的方法,该方法符合预期目的。
{"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 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-26 DOI: 10.1093/jaoacint/qsae064
Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise
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.
背景 美国国家标准与技术研究院(NIST)已生产出 40 多种植物膳食补充剂标准物质® (SRM) 和参考物质 (RM),并对化学标记和/或活性化合物进行了赋值。虽然有毒元素(砷、镉、铅和汞)的环境累积或无意引入是植物膳食补充剂产品的潜在暴露源,但大多数膳食补充剂标准物质/标准参考物质都没有为这四种主要有毒元素赋值。目标 确定 NIST 植物膳食补充剂 SRM/RM 现有库存中的砷、镉、铅和汞含量。方法 利用硝酸微波辅助消解法分析植物部分、提取物和成品[即固体口服剂型 (SODF)]的 15 个 SRMs/RMs 套件中的砷、镉、铅和汞含量,然后利用电感耦合等离子体质谱法进行定量。结果 对照样品的结果与认证值十分吻合,表明对 38 个植物 SRM/RM 的分析处于受控状态。对来自同一来源材料的相关植物/提取物 SRM/RM 的表征表明,虽然萃取过程通常会使提取物中汞或砷的有毒元素含量降低,但也有可能在萃取后质量分数水平保持不变,甚至有所增加。结论 这些结果填补了 SRMs/RMs 毒性元素含量范围方面的重大知识空白,因为 NIST 并没有为 SRMs/RMs 赋值,尤其是汞含量以及萃取物和 SODF 基质。现在有了全面的有毒元素含量,研究人员就能更好地选择适当的膳食补充剂 SRM/RM,在膳食补充剂成分和产品分析中用作对照。亮点 报告了 38 种膳食补充剂 SRM/RM(包括 6 套植物、提取物和 SODF 以及 9 对来自同一批植物材料的植物和提取物)的砷、镉、铅和汞含量结果。
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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 Q2 Medicine Pub Date : 2024-04-30 DOI: 10.1093/jaoacint/qsae039
Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz
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.
背景 含腐植酸(HA)和富里酸(FA)的产品具有巨大的商业潜力,然而,消费者并不知道,有些产品可能贴错标签或含有掺假物。贴错标签和掺假的情况主要出现在富里酸产品中。使用紫外可见光谱来区分真假 FA 产品既实用又可取。本研究的目的是扩大使用 Mayhew 等人 2023 年提出的基于紫外可见光谱的方法生成的数据集。方法 使用 Mayhew 等人,2023 年提出的紫外-可见光方法(在本研究中称为 UVAC(紫外吸光度确认)方法),总共使用了三十(30)个测试样本来生成九十个测试部分(每个测试样本 3 个重复)进行分析。结果 在所调查的 13 个 FA 测试样品中,没有一个样品被确定为使用紫外吸光度确认法进行的腐殖化。所研究的 FA 样品包括两种 IHSS 标准、五种商业 FA 产品 (CFAP) 和六种全 FA 馏分 (SFA),它们是从六种已知的固体腐殖质材料来源 (SHMS) 中分离出来的。其中有一种柠檬岩、一种腐植岩和四种泥炭来源被用作 SHMS。对 SHMS 的中和提取物进行分析后发现,只有 3/6 的 SHMS 被确定为腐殖质。通过分离 SHMS 中的 HA,还生成了 6 个 HA(SHA)测试样本,结果只有 3/6 的 SHA 被确定为腐殖化。结论 鉴于错误测定的发生率较高,需要进一步改进该方法,以便供行业或监管机构使用。要点 建议的方法未能确定 IHSS FA 标准为腐殖化。虽然该方法很实用,但还需要改进和进一步研究,才能用于可靠地区分真假 FA 或 HA。
{"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 Q2 Medicine Pub Date : 2024-04-25 DOI: 10.1093/jaoacint/qsae037
Renuka P Rathnasekara, Jingzhi Tian, A. M. Rustum
BACKGROUNDThe topical veterinary drug product containing fipronil and permethrin provides an effective repellent protection and high insecticidal efficacy for dogs.OBJECTIVEThe 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.METHODThe 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.RESULTSSpecificity 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.CONCLUSIONSHere, 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.HIGHLIGHTSThe new HPLC method permits the acquisition of data for all analytes of interest for a topical finished drug product containing fipronil, permethrin, and BHT.
背景含有氟虫腈和氯菊酯的外用兽药产品可为狗提供有效的驱虫保护和较高的杀虫效果。目的本研究旨在开发一种稳定性指示高效液相色谱 (HPLC) 方法,用于同时检测和定量外用兽药产品中的氟虫腈和氯菊酯及其主要降解产物和丁基羟基甲苯 (BHT)。方法 采用 Phenomenex Kinetex C18 色谱柱(150 × 3 mm,粒径 2.6 µm),以 H2O/acetonitrile/isopropyl alcohol/85% H3PO4 (65.5 + 32.5 + 4/0.0053, v/v/v/v)为流动相-A,乙腈(100%)为流动相-B,在 37 °C 下进行梯度洗脱,分离两种活性成分、其降解产物和抗氧化剂(BHT)。结果在强制降解的成品中,氟虫腈、氯菊酯及其降解产物和 BHT 得到了充分的分离,证明了该方法的特异性。该方法的线性范围为两种活性成分目标分析浓度的 0.2% 至 150%,BHT 为 50%至 150%。在线性范围内,安慰剂添加的活性成分溶液中氟虫腈、氯菊酯和 BHT 的回收率极高,表明该方法具有足够的准确性。该方法的 LOQ 和 LOD 分别为分析浓度的 0.2% 和 0.07%。结论在此,我们报告了一种稳健、具有稳定性指示的高效液相色谱法的开发和验证情况,该方法可用于氟虫腈、氯菊酯和 BHT 的鉴定和检测,包括狗用外用药物产品中氟虫腈和氯菊酯降解产物的估计。亮点新的高效液相色谱法可以获得含有氟虫腈、氯菊酯和 BHT 的外用药物成品中所有相关分析物的数据。
{"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 Q2 Medicine Pub Date : 2024-04-23 DOI: 10.1093/jaoacint/qsae035
Ibrahim A Darwish, Nourah Z. Alzoman, M. S. Alsalhi
BACKGROUNDTulathromycin (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.OBJECTIVESThe aim of this study was the development of two innovative microwell spectrophotometric methods (MW-SPMs) for determination of TUL in its pharmaceutical bulk form.METHODSThe 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.RESULTSThe 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.CONCLUSIONSThis study described two new MW-SPMs as valuable analytical tools for the determination of TUL.
背景图拉霉素(TUL)是一种三酰氨基苯胺类抗菌药,已被欧盟和美国批准用于治疗和预防牛呼吸道疾病。本研究旨在开发两种创新的微孔分光光度法(MW-SPMs),用于测定药用散装 TUL。方法以 2,5-二羟基-3,6-二氯环己-2,5-二烯-1,4-二酮(HCD)和 2,3-二氯-5,6-二氰基对苯醌(CBQ)为π电子受体,研究了作为电子供体的 TUL 的电荷转移复合物(CTC)的形成。利用紫外-可见分光光度法和计算对四氯化碳进行了表征。结果四氯化碳的形成是通过与 HCD 和 CBQ 的四氯化碳分别在 520 nm 和 460 nm 处形成最大吸收的特征吸收带来证实的。两种四氯化碳的化学计量比均为 1:1,不同光谱常数和电子常数的值证实了四氯化碳的稳定性。推测了反应的机理。两种 MW-SPM 的线性范围均为 10-500 µg/mL。涉及与 HCD 和 CBQ 反应的方法的定量限分别为 13.5 和 26.4 微克/毫升。这两种方法都成功地应用于散装药物中 TUL 的定量分析,准确度和精密度均可接受。生态友好/绿色评估结果证明,这两种 MW-SPM 均符合绿色分析方法的要求。此外,这些方法一步反应,同时处理大量微量样品,具有高通量分析的优势。
{"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 Q2 Medicine 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
BACKGROUNDCassia (Family: Fabaceae) species are a large group of flowering plants rich in bioactive anthraquinone and flavonoids used in botanical supplements and nutraceuticals.OBJECTIVEA 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.METHODAll 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.RESULTSThe 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.CONCLUSIONSThe 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.HIGHLIGHTSThis 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.
背景决明(科:豆科)是一大类开花植物,富含生物活性蒽醌和黄酮类化合物,可用于植物补充剂和营养保健品。采用基于液相色谱的电喷雾质谱(ESI-MS/MS)方法进一步确认了这些化合物在所选决明树种的叶和花中的含量。采用 Zorbax TC18(4.6 x 250,粒径 5 μm)分析柱,以 0.1% 甲酸和乙腈为洗脱溶剂,流速为 0.8 mL/min,检测波长为 259 nm。对于 HPTLC 指纹分析,优化了甲苯、乙酸乙酯和甲酸(5.5:4.2:0.6, v/v/v)的流动相组成,使用硅胶 60F254 铝板分离和鉴定所有化合物。结果所开发的 HPLC-PDA 方法对 13 种化合物的验证数据显示线性关系良好(r2 > 0.99),灵敏度为 LOD(0.082-1.969 mg/mL)、LOQ(0.250-5.967 mg/mL),回收率为 85.22%-100.32%。经ESI-MS/MS确认,决明子样品中的定量结果为-0.77-0.44,精确度高(相对误差小于5.0%)。结论:所开发的 HPLC-PDA 方法简单、精确,可分离和定量蒽醌类化合物和黄酮类化合物,并可使用基于新型 LC 的 ESI-MS/MS 进行确认。该新型多平台方法采用数据整合策略,成功地同时鉴定和定量了七种具有重要药用价值的决明子叶和花中的十三种化合物。
{"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 Q2 Medicine 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
BACKGROUNDEstimation 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.OBJECTIVEThe 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.METHODSTo 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.RESULTSThe 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.CONCLUSIONThe 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.HIGHLIGHTSThe 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.
背景药物的估计和方法的开发是制剂开发的一个重要方面,也是分析科学家的一个关键因素。为了简化吉非替尼等溶解性较差的药物的估算,采用了响应面方法(RSM),并有效利用盒-贝肯设计(BBD)模型来获得精确的计算设计空间。筛选了 3 个主要的混合效应独立因素(缓冲液百分比、缓冲液 pH 值和流速)和 3 个突出的因果反应(即理论平板、保留时间和尾流因子),以进行优化分析。结果该 RP-HPLC 方法采用了质量源于设计(QbD)的方法,能在 4.5 分钟内有效地估算出分析物的浓度。所开发的方法经济稳健、灵敏度高,所有选定验证参数的相对标准偏差(%RSD)均小于 2%。估计的设计空间表明,在流动相缓冲液含量为 60%、pH 值为 4.25、流速为 0.7 mL/min 时,该方法的可取性最高(R2-0.998)。该分析方法采用质量源于设计的方法进行设计和量化,使 RP-HPLC 方法更加稳健高效,可用于复杂纳米制剂中分析物的估算。此外,该方法还可通过协同处理步骤消除估算过程中的干扰分子。所开发的方法节省了时间和溶剂成本,并采用了最近监管部门关注的 QbD 要求。
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Journal of AOAC International
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