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Stability and Biosimilarity Assessment of Bevacizumab Monoclonal Antibody; Orthogonal Testing Protocol Coupled With Peptide Mapping-Principal Component Analysis. 贝伐单抗单克隆抗体的稳定性和生物相似性评估;结合肽图谱--主要成分分析的正交测试方案。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad094
Sara H Abdelghaffar, Maha A Hegazy, Basma M Eltanany

Background: Biologics are essential in cancer treatment because they stimulate the body's natural response to fight cancer, but they are expensive. Biosimilars are more affordable compared to patent biologicals, but it must be verified that they are as effective as their innovators. Characterization of biosimilars and assessment of interchangeability requires many data points for verification.

Objective: The proposed study provides a quality assessment of two new bevacizumab (BVZ) biosimilars, produced by Amgen and Biocad, Inc., through the development and greenness assessment of an orthogonal testing protocol and purity indicating assay, including size-exclusion (SE-HPLC), reversed-phase (RP-HPLC), and cation exchange chromatography (CEX-HPLC) in addition to dynamic light scattering (DLS) and sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE).

Methods: SE-HPLC method was performed and validated to screen the BVZ monomer and its aggregates and/or fragments. Peak purity and system suitability parameters were calculated. Results indicate that the orthogonal protocol is a useful tool for assessing monoclonal antibody stability. It is a key criterion for biosimilarity assessment. DLS and SDS-PAGE results were compared to each other to reveal close retention times and banding patterns between BVZ innovator and its biosimilars. These results showed that Avastin® and the investigated biosimilars have the same profile in terms of peak area of related compounds within the acceptance limit and apparent molecular weight, and the SDS-PAGE technique was found to be the most eco-friendly technique among others.

Conclusions: The results obtained highlighted the importance of assessing similarities and differences in ensuring the biosimilarity and interchangeability of the studied products.

Highlights: BVZ is one of the essential monoclonal antibodies in the treatment of colorectal cancer (CRC). BVZ biosimilars were evaluated by developing an orthogonal testing protocol and a purity-indicating assay. The size-exclusion (SE)-HPLC method was applied and validated to monitor the BVZ monomer and its aggregates. The results demonstrated the importance of assessing the stability and biosimilarity of BVZ.

背景:生物制剂在癌症治疗中至关重要,因为它们能刺激人体的自然反应来对抗癌症,但价格昂贵。与专利生物制剂相比,生物仿制药更经济实惠,但必须验证它们是否与创新药一样有效。生物仿制药的特征描述和互换性评估需要许多数据点来验证:拟议的研究将对安进公司和百奥凯公司生产的两种新型贝伐单抗(BVZ)生物仿制药进行质量评估、方法:采用SE-HPLC、RP-HPLC和阳离子交换色谱法(CEX-HPLC)以及动态光散射法(DLS)和十二烷基硫酸钠-聚丙烯酰胺凝胶电泳法(SDS-PAGE)对安进公司和Biocad公司生产的两种新型贝伐珠单抗(BVZ)生物仿制药进行质量评估:采用 SE-HPLC 方法筛选 BVZ 单体及其聚集体和/或片段,并进行了验证。计算了峰纯度和系统适用性参数。结果表明,正交方案是评估单克隆抗体稳定性的有效工具。它是生物相似性评估的一个关键标准。通过比较 DLS 和 SDS-PAGE 结果,发现 BVZ 创新药与其生物仿制药的保留时间和条带模式非常接近。这些结果表明,阿瓦斯汀®和所研究的生物仿制药在相关化合物的峰面积和表观分子量方面具有相同的特征,而且发现 SDS-PAGE 技术是最环保的技术:结论:研究结果表明,在确保所研究产品的生物相似性和互换性时,对其异同点进行评估非常重要:BVZ是治疗结直肠癌(CRC)的重要单克隆抗体之一。通过制定正交试验方案和纯度指示测定法,对BVZ生物仿制药进行了评估。应用并验证了尺寸排阻(SE)-HPLC方法来监测BVZ单体及其聚集体。结果表明了评估 BVZ 的稳定性和生物相似性的重要性。
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引用次数: 0
Green HPLC Method for Simultaneous Analysis of Three Natural Antioxidants by Analytical Quality by Design. 通过 "分析质量源于设计 "实现同时分析三种天然抗氧化剂的绿色高效液相色谱法。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad105
Ramya Jonnalagadda, Seetharaman Rathinam, Krishnaveni Nagappan, Vinodhini Chandrasekar

Background: Glutathione, silybin, and curcumin are well-known potential antioxidants that are recommended as adjuvant therapy in cancer treatment.

Objective: Based on the principles of Analytical Quality by Design (AQbD) and green analytical chemistry, a simple, robust, and environmentally benign HPLC method for the simultaneous estimation of glutathione, silybin, and curcumin in bulk and formulation was performed.

Method: Elution was achieved by an Agilent Eclipse XDB C18 (150 mm × 4.6 mm id, 3.5 μm) column using a gradient mobile phase composed of ethanol-water pH 6.7 (with 0.1%, v/v orthophosphoric acid) and 1.07 mL/min flow rate with PDA detection at 215 nm. Critical method variables were identified by risk assessment using an Ishikawa diagram, and multivariate optimization of the experimental conditions for the HPLC technique was accomplished by central composite design using design of experiments (DoE) software.

Results: The separation was achieved within 15 min, where the retention time of glutathione, silybin, and curcumin were 3.3, 4.9, and 7.3 min, respectively. The standard curve was linear in the range of 3.75-26.25 µg/mL for glutathione, 62.50-437.50 µg/mL for silybin, and 12.5-87.50 µg/mL for curcumin. The developed method was validated as per ICH guidelines Q2 (R1), and all the parameters are within specified limits.

Conclusions: The proposed method is simple, precise, and robust, which can be employed for routine analysis and also concluded to be a greener approach according to AGREE, Green Analytical Procedure Index, and analytical eco-scale tools.

Highlights: The chosen antioxidants were evaluated for the very first time simultaneously using the chromatographic technique in bulk and dosage forms employing green solvents. The peak purity of all three compounds was studied using a PDA detector. Wastage was reduced in terms of time, cost, and solvents by employing AQbD elements and tools. Complete application of environmentally sustainable safe solvents were employed.

背景:谷胱甘肽、水飞蓟素和姜黄素是众所周知的潜在抗氧化剂,被推荐作为癌症治疗的辅助疗法:基于设计分析质量(AQbD)和绿色分析化学的原则,建立了一种简单、稳健、对环境无害的高效液相色谱法,用于同时测定散装和制剂中的谷胱甘肽、水飞蓟素和姜黄素:采用Agilent Eclipse XDB C18 (150 mm × 4.6 mm id, 3.5 μm)色谱柱,以pH 6.7的乙醇-水(含0.1% v/v正磷酸)为流动相梯度洗脱,流速为1.07 mL/min,在215 nm波长下进行PDA检测。通过使用石川图进行风险评估,确定了关键的方法变量,并使用实验设计(DoE)软件通过中心复合设计对高效液相色谱技术的实验条件进行了多变量优化:谷胱甘肽、水飞蓟素和姜黄素在 15 分钟内实现分离,保留时间分别为 3.3、4.9 和 7.3 分钟。谷胱甘肽、水飞蓟素和姜黄素在3.75-26.25微克/毫升、62.50-437.50微克/毫升和12.5-87.50微克/毫升范围内线性关系良好。根据 ICH 指南 Q2 (R1),对所开发的方法进行了验证,所有参数均在规定的范围内:结论:所提出的方法简单、精确、稳健,可用于常规分析,根据 AGREE、绿色分析程序指数和分析生态尺度工具,该方法是一种更环保的方法:首次使用色谱技术同时评估了所选抗氧化剂在使用绿色溶剂的散装和剂型中的应用。使用 PDA 检测器研究了所有三种化合物的峰纯度。通过使用 AQbD 元素和工具,减少了时间、成本和溶剂方面的浪费。完全采用了环境可持续的安全溶剂。
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引用次数: 0
Smart Multivariate Spectrophotometric Determination of Two Co-Administered Autoimmune Drugs; Sulfasalazine and Pentoxifylline; in Bulk and Spiked Human Plasma. 智能多变量分光光度法测定散装和加标人体血浆中两种联合用药的自身免疫性药物:磺胺沙拉嗪和喷托西林。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad097
Maimana A Magdy, Nehal F Farid, Basma H Anwar, Nessreen S Abdelhamid

Background: Sulfasalazine and pentoxifylline are co-prescribed together to treat psoriasis and pemphigus vulgaris. Sulfasalazine is an anti-inflammatory, immunosuppressant, and antibiotic drug, while pentoxifylline is a vasodilator and immunosuppressant. The spectra of the two drugs and plasma suffer from severe overlap.

Objective: This work aims to simultaneously determine sulfasalazine and pentoxifylline in their binary mixture and spiked human plasma by the assessment of their UV spectral data.

Methods: Two model updated chemometric methods were established using principal component regression and partial least-squares regression models. The two models were validated in accordance with the U.S. Food and Drug Administration guidelines for bioanalysis and were applied for the determination of both drugs in synthetic mixtures or spiked human plasma.

Results: Accuracy and precision were within the accepted limits. In addition, three different assessment methods were used to evaluate the environmental greenness of the proposed models.

Conclusion: The two updated models are simple, rapid, sensitive, and precise, and could be easily applied in QC laboratories for determination of sulfasalazine and pentoxifylline, without any preliminary separation steps or interference from plasma matrix.

Highlights: Two updated chemometric models called principlal component regression and partial least-squares regression were established for determination of sulfasalazine and pentoxifylline in spiked human plasma using UV spectrophotometric data.

背景:磺胺沙拉嗪和喷托昔林可同时用于治疗银屑病和寻常型天疱疮。磺胺二甲嘧啶是一种抗炎药、免疫抑制剂和抗生素,而喷昔利林是一种血管扩张剂和免疫抑制剂。这两种药物和血浆的光谱存在严重重叠:本研究旨在通过评估两种药物的紫外光谱数据,同时测定其二元混合物和加标人体血浆中的柳氮磺胺吡啶和喷托非福林:方法: 利用主成分回归和偏最小二乘回归模型,建立了两种模型更新的化学计量学方法。根据美国食品和药物管理局的生物分析指南对这两个模型进行了验证,并将其应用于合成混合物或加标人体血浆中两种药物的测定:结果:准确度和精密度均在可接受的范围内。此外,还采用了三种不同的评估方法来评价所提议模型的环保性:结论:这两个更新的模型简单、快速、灵敏、精确,可轻松应用于质控实验室中磺胺沙拉嗪和喷昔利嗪的测定,无需任何初步分离步骤,也不会受到血浆基质的干扰:利用紫外分光光度法数据建立了两个新的化学计量模型,分别称为原理成分回归模型和部分最小二乘回归模型,用于测定加标人体血浆中的磺胺沙拉嗪和喷昔利嗪。
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引用次数: 0
A Simple UV Spectrophotometric Method Based on Continuous Wavelet Transform and Multivariate Calibration Model for the Concurrent Analysis of Three Water-Soluble Vitamins in Fertility Supplements. 基于连续小波变换和多元校准模型的简单紫外分光光度法,用于同时分析生育保健品中的三种水溶性维生素。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad093
Mahla Lohrdy, Mahmoud Reza Sohrabi, Mehran Davallo

Background: Owing to the presence of overlapping spectra in pharmaceutical components, classical spectrophotometry is hard for concurrent determination. The advance of chemometrics along with UV-Vis spectrophotometry has contributed to solving this problem.

Objective: In this study, a fast, easy, precise, accurate, low-cost, and eco-friendly spectrophotometric technique was introduced and validated for the simultaneous analysis of vitamin B6, vitamin B12, and vitamin C in fertility supplements for men and women using continuous wavelet transform (CWT) and partial least squares (PLS) techniques without using time-consuming extraction process and organic solvents.

Method: In the CWT method, the zero-crossing technique was applied to obtain the optimum points for plotting calibration curves for each component. The validation of both methods was evaluated by analyzing several mixtures with different concentrations. The efficiency of the proposed methods was also surveyed on commercial capsules.

Results: Wavelet families, including Symlet (sym2) at 230, Biorthogonal (bior1.3) at 378 nm, and Daubechies (db2) at 261, were considered for vitamins B6, B12, and C, respectively. The linear range was found to be 8-20, 8-20, and 10-25 μg/mL with the coefficient of determination (R2) equal to 0.9982, 0.9978, and 0.9701 for B6, B12, and C, respectively. Low limit of detection (LOD) (<0.09 μg/mL) and limit of quantification (LOQ) <0.9 μg/mL were achieved. The mean recovery values in synthetic mixtures were from 98.38 to 98.89% and from 99.83 to 99.99%, where root-mean-square error (RMSE) of not more than 0.4 and 0.05 using the CWT and PLS methods, respectively.

Conclusions: The obtained results from the commercial capsules, applying the suggested techniques, were compared to those yielded by the high-performance liquid chromatography (HPLC) method using the analysis of variance (ANOVA) test. According to the results, there are no significant differences, and they were in good agreement. According to all the mentioned cases, the proposed approaches can replace the time-consuming and costly HPLC method in quality control laboratories.

Highlights: Green spectrophotometry coupling chemometrics methods were proposed. Simultaneous determination of three water-soluble vitamins in fertility supplements was done using these approaches. Rapidity, simplicity, low cost, and accuracy are the benefits of the proposed methods. A HPLC technique was used as a reference method to compare with the chemometrics methods.

背景:由于药物成分中存在重叠光谱,传统的分光光度法很难同时进行测定。化学计量学和紫外可见分光光度法的发展有助于解决这一问题:本研究采用连续小波变换(CWT)和偏最小二乘法(PLS)技术,在不使用耗时的提取过程和有机溶剂的情况下,引入并验证了一种快速、简便、精确、低成本且环保的分光光度法,用于同时分析男性和女性生育保健品中的维生素 B6、维生素 B12 和维生素 C:方法:在 CWT 方法中,应用零交叉技术来获得绘制各成分校准曲线的最佳点。通过分析几种不同浓度的混合物,对这两种方法的有效性进行了评估。此外,还对商用胶囊的效率进行了调查:对维生素 B6、B12 和 C 分别采用了小波系列,包括 230 纳米波长的 Symlet (sym2)、378 纳米波长的 Biorthogonal (bior1.3) 和 261 纳米波长的 Daubechies (db2)。结果发现,维生素 B6、维生素 B12 和维生素 C 的线性范围分别为 8-20、8-20 和 10-25 μg/mL,测定系数 (R2) 分别为 0.9982、0.9978 和 0.9701。检测限(LOD)较低(结论):通过方差分析(ANOVA)测试,将采用建议的技术从商品胶囊中获得的结果与高效液相色谱法(HPLC)获得的结果进行了比较。结果表明,二者没有明显差异,一致性良好。根据上述所有情况,所提出的方法可以在质量控制实验室中取代费时费力的高效液相色谱法:提出了绿色分光光度法耦合化学计量学方法。亮点:提出了绿色分光光度法耦合化学计量学方法,利用这些方法同时测定了生育补充剂中的三种水溶性维生素。所提方法具有快速、简便、低成本和准确等优点。使用高效液相色谱技术作为参考方法,与化学计量学方法进行比较。
{"title":"A Simple UV Spectrophotometric Method Based on Continuous Wavelet Transform and Multivariate Calibration Model for the Concurrent Analysis of Three Water-Soluble Vitamins in Fertility Supplements.","authors":"Mahla Lohrdy, Mahmoud Reza Sohrabi, Mehran Davallo","doi":"10.1093/jaoacint/qsad093","DOIUrl":"10.1093/jaoacint/qsad093","url":null,"abstract":"<p><strong>Background: </strong>Owing to the presence of overlapping spectra in pharmaceutical components, classical spectrophotometry is hard for concurrent determination. The advance of chemometrics along with UV-Vis spectrophotometry has contributed to solving this problem.</p><p><strong>Objective: </strong>In this study, a fast, easy, precise, accurate, low-cost, and eco-friendly spectrophotometric technique was introduced and validated for the simultaneous analysis of vitamin B6, vitamin B12, and vitamin C in fertility supplements for men and women using continuous wavelet transform (CWT) and partial least squares (PLS) techniques without using time-consuming extraction process and organic solvents.</p><p><strong>Method: </strong>In the CWT method, the zero-crossing technique was applied to obtain the optimum points for plotting calibration curves for each component. The validation of both methods was evaluated by analyzing several mixtures with different concentrations. The efficiency of the proposed methods was also surveyed on commercial capsules.</p><p><strong>Results: </strong>Wavelet families, including Symlet (sym2) at 230, Biorthogonal (bior1.3) at 378 nm, and Daubechies (db2) at 261, were considered for vitamins B6, B12, and C, respectively. The linear range was found to be 8-20, 8-20, and 10-25 μg/mL with the coefficient of determination (R2) equal to 0.9982, 0.9978, and 0.9701 for B6, B12, and C, respectively. Low limit of detection (LOD) (<0.09 μg/mL) and limit of quantification (LOQ) <0.9 μg/mL were achieved. The mean recovery values in synthetic mixtures were from 98.38 to 98.89% and from 99.83 to 99.99%, where root-mean-square error (RMSE) of not more than 0.4 and 0.05 using the CWT and PLS methods, respectively.</p><p><strong>Conclusions: </strong>The obtained results from the commercial capsules, applying the suggested techniques, were compared to those yielded by the high-performance liquid chromatography (HPLC) method using the analysis of variance (ANOVA) test. According to the results, there are no significant differences, and they were in good agreement. According to all the mentioned cases, the proposed approaches can replace the time-consuming and costly HPLC method in quality control laboratories.</p><p><strong>Highlights: </strong>Green spectrophotometry coupling chemometrics methods were proposed. Simultaneous determination of three water-soluble vitamins in fertility supplements was done using these approaches. Rapidity, simplicity, low cost, and accuracy are the benefits of the proposed methods. A HPLC technique was used as a reference method to compare with the chemometrics methods.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"164-176"},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10414983","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 Chromatographic Estimation of Vildagliptin and Dapagliflozin Using Hybrid Principles of White Analytical Chemistry and Analytical Quality by Design. 利用白分析化学和设计分析质量的混合原理同时色谱法估算维达列汀和达帕格列汀
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad108
Pintu Prajapati, Bageshree Rana, Veera Shakar Pulusu, Shailesh Shah

Background: The fixed-dose combination of vildagliptin (VDG) and dapagliflozin (DGZ) is used in the treatment of type 2 diabetes mellitus. According to the literature survey, RP-HPLC and HPTLC methods have been reported for routine analysis of VDG and DGZ. These chromatographic methods have been developed using potentially neurotoxic and teratogenic solvents, which are unsafe for human and aquatic animal life and hazardous to the environment. These types of organic solvents shall be replaced or reduced during chromatographic analysis of drugs for the safety of human and aquatic animal life and the protection of the environment. The novel white analytical chemistry (WAC) approach has been introduced, which emphasizes robust, green, user-friendly, economical, and rapid analysis of drug samples.

Objective: Hence, the WAC-based RP-HPLC method has been developed for the estimation of VDG and DGZ using lower toxic and economical solvents.

Method: The development of the RP-HPLC method includes the implementation of the analytical quality by design approach using principles of design of experiments to reduce organic waste generation and regulatory compliance of analytical method. The central composite design was applied for response surface modeling (RSM) and optimization of the RP-HPLC method. The method validation was carried out according to ICH Q2 (R1) guidelines.

Results: The fixed-dose combinations of VDG and DGZ were assayed, and results were found in compliance with their labeled claim. The published and proposed RP-HPLC methods were assessed for chromatographic analysis of VDG and DGZ using the Red-Green-Blue (RGB) model, AGREE calculator, Eco-Scale Assessment tool, GAPI software, and NEMI standards.

Conclusions: The proposed method was found to be robust, green, economical, and user-friendly for chromatographic analysis of VDG and DGZ. The proposed method can be an economical and eco-friendly analytical tool in the pharmaceutical industry for quality control and routine analysis of fixed-dose combinations of VDG and DGZ.

Highlights: Hybrid principles of WAC and analytical quality by design to RP-HPLC method for simultaneous estimation of VDG and DGZ in their fixed-dose combinations.

背景:维达列汀(VDG)和达帕格列净(DGZ)的固定剂量复方制剂用于治疗2型糖尿病。根据文献调查,目前已有用于常规分析 VDG 和 DGZ 的 RP-HPLC 和 HPTLC 方法的报道。这些色谱法使用的溶剂可能具有神经毒性和致畸性,对人类和水生动物的生命不安全,而且对环境有害。为了人类和水生动物的生命安全和保护环境,在对药物进行色谱分析时,应替换或减少这些类型的有机溶剂。因此,我们开发了基于白分析化学(WAC)的 RP-HPLC 方法,使用毒性较低且经济的溶剂来估算 VDG 和 DGZ:方法:RP-HPLC 方法的开发包括利用实验设计原则实施分析质量设计方法,以减少有机废物的产生并使分析方法符合法规要求。中心复合设计用于响应面建模(RSM)和 RP-HPLC 方法的优化。根据 ICH Q2 (R1) 指南进行了方法验证:结果:对VDG和DGZ的固定剂量复方制剂进行了检测,结果符合其标签要求。采用红-绿-蓝(RGB)模型、AGREE 计算器、生态尺度评估工具、GAPI 软件和 NEMI 标准,对已公布和拟议的 RP-HPLC 方法进行了评估,以对 VDG 和 DGZ 进行色谱分析:结论:所提出的方法在色谱分析 VDG 和 DGZ 方面具有稳健、绿色、经济和用户友好的特点。结论:所提出的方法在 VDG 和 DGZ 固定剂量复方制剂的色谱分析中具有稳健性、绿色性、经济性和用户友好性,可作为制药行业中一种经济、环保的分析工具,用于质量控制和常规分析:将WAC和分析质量的混合原理应用于RP-HPLC方法,用于同时估算VDG和DGZ的固定剂量复方制剂。
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引用次数: 0
Development and Validation of a Method for Trace Level Zinc Quantification in Pharmaceutical Zinc Supplements Using a Carboxyl Functional Group Packed Column and Refractive Index Detector. 利用羧基官能团填料色谱柱和折射率检测器开发并验证药用锌补充剂中痕量锌定量方法
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad101
Nagavardhana Reddy Vanga, Venkata Ratnam Kesamsetty, Kumaraswamy Ummiti, Venkata Nadh Ratnakaram, Hanimi Reddy Bapatu

Background: Zinc helps with cell division, growth, wound healing, and carbohydrate breakdown. Humanbeings have to obtain zinc from food or supplements because our bodies do not produce it naturally. In view of the greater advantages (such as low cost, time of analysis, and stability-indicating) compared to other quantification methods (titration, ion chromatography, Atomic absorption spectroscopy) proposed in the literature, a refractive index detector coupled with HPLC has been used in quantification of zinc.

Objective: The goal of this research is to develop and validate a sensitive, low-cost, high-resolution, and stability- indicating method for detecting and quantifying zinc levels in zinc supplement pharmaceutical products (injectables, tablets, and capsules).

Methods: A novel isocratic reverse-phase HPLC method with a refractive index detector (with sensitivity 64, detector temperature 35°C, and positive polarity) was developed using a carboxyl functional group packed column and 0.8% (v/v) formic acid as the mobile phase to detect and quantify zinc content.

Results: The reported method has a good optimal sensitivity (LOQ: 0.006 mg/mL and LOD: 0.002 mg/mL). The correlation coefficient (r) obtained from the zinc calibration plot was greater than 0.998, indicating that the method was linear and that there was a strong correlation between zinc concentration (0.006 mg/mL to 0.375 mg/mL) and peak response. The accuracy at LOQ level was found to be 95-105% and 97-103% at the remaining levels (50, 100, and 150%).

Conclusion: The proposed method was successfully developed and validated as per International council for harmonisation (ICH) guidelines. Therefore, this method can be used for the quantitative testing of zinc in the QC laboratory.

Highlights: A novel method was developed for zinc levels determination in pharmaceutical products using HPLC with a refractive index detector. The present approach has a quick run time of 10 min and is inexpensive.

背景:锌有助于细胞分裂、生长、伤口愈合和碳水化合物分解。人类必须从食物或补充剂中获取锌,因为我们的身体不能自然产生锌。与文献中提出的其他定量方法(滴定法、离子色谱法、原子吸收光谱法)相比,折射率检测器结合高效液相色谱法具有更大的优势(如成本低、分析时间短、指示稳定):本研究的目标是开发和验证一种灵敏、低成本、高分辨率和稳定性指示的方法,用于检测和定量补锌药品(注射剂、片剂和胶囊)中的锌含量:方法:采用羧基官能团填料色谱柱,以 0.8% (v/v) 甲酸为流动相,建立了一种新型等度反相高效液相色谱法,该方法采用折光检测器(灵敏度为 64,检测器温度为 35°C,极性为正)检测和定量锌的含量:报告的方法具有良好的最佳灵敏度(LOQ:0.006 mg/mL,LOD:0.002 mg/mL)。锌校准图的相关系数(r)大于 0.998,表明该方法线性良好,锌浓度(0.006 毫克/毫升至 0.375 毫克/毫升)与峰值响应之间有很强的相关性。LOQ水平的准确度为95-105%,其余水平(50%、100%和150%)的准确度为97-103%:根据国际协调理事会(ICH)的指导方针,成功开发并验证了所提出的方法。因此,该方法可用于质控实验室的锌定量检测:利用高效液相色谱法和折射率检测器,开发了一种测定药品中锌含量的新方法。该方法运行时间短,仅需 10 分钟,且成本低廉。
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引用次数: 0
Detection of the Adulteration of Dendrobium Huoshanense with Dendrobium Henanense by UV-Vis-Shortwave Near-Infrared Diffuse Reflectance Spectroscopy Combined with Chemometrics. 紫外-可见-短波近红外漫反射光谱与化学计量学相结合检测霍山石斛与河南石斛的掺假。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad090
Jing-Wen Hao, Nai-Dong Chen, Xiao-Quan Liu, Qiang Li, Hui-Min Xu, Wei-Han Yang, Chao-Feng Qin, Ya-Qing Bu

Background: Dendrobium huoshanense (DHS) is a classic traditional Chinese medicine (TCM) with distinctive medicinal benefits and great economic worth; nevertheless, because of similar tastes and looks, it is simple to adulterate with less expensive substitutes (such as Dendrobium henanense [DHN]).

Objective: This work aimed to develop a reliable tool to detect and quantify the adulteration of DHS with DHN by using UV-Vis-shortwave near-infrared diffuse reflectance spectroscopy (UV-Vis-SWNIR DRS) combined with chemometrics.

Methods: Adulterated samples prepared in varying concentrations (0-100%, w/w) were analyzed with UV-Vis-SWNIR DRS methods. Partial least-square-discriminant analysis (PLS-DA) and partial least-squares (PLS) regression techniques were used for the differentiation of adulterated DHN from pure DHS and the prediction of adulteration levels.

Results: The PLS-DA classification models successfully differentiated adulterated and nonadulterated DHS with an over 100% correct classification rate. UV-Vis-SWNIR DRS data were also successfully used to predict adulteration levels with a high coefficient of determination for calibration (0.9924) and prediction (0.9906) models and low error values for calibration (3.863%) and prediction (5.067%).

Conclusion: UV-Vis-SWNIR DRS, as a fast and environmentally friendly tool, has great potential for both the identification and quantification of adulteration practices involving herbal medicines and foods.

Highlights: UV-Vis-SWNIR DRS combined with chemometrics can be applied to identify and quantify the adulteration of herbal medicines and foods.

背景:霍山石斛(Dendrobium huoshanense,DHS)是一种经典的传统中药,具有独特的药用价值和巨大的经济价值;然而,由于口味和外观相似,很容易掺入价格较低的替代品(如河南石斛[Dendrobium henanense [DHN]):本研究旨在开发一种可靠的工具,利用紫外可见短波近红外漫反射光谱(UV-Vis-SWNIR DRS)结合化学计量学方法,检测和量化 DHS 与 DHN 的掺假情况:采用紫外可见-短波近红外扩散反射光谱法(UV-Vis-SWNIR DRS)对不同浓度(0-100%,w/w)的掺假样品进行分析。采用偏最小二乘判别分析(PLS-DA)和偏最小二乘回归技术来区分掺假的 DHN 和纯 DHS,并预测掺假程度:结果:PLS-DA 分类模型成功区分了掺假和未掺假的 DHS,分类正确率超过 100%。紫外可见-西可见-近红外 DRS 数据也成功用于预测掺假水平,定标(0.9924)和预测(0.9906)模型的确定系数较高,定标(3.863%)和预测(5.067%)的误差值较低:结论:紫外可见-西可见近红外 DRS 作为一种快速、环保的工具,在识别和量化中药材和食品掺假行为方面具有巨大潜力:亮点:紫外-可见-全可见-近红外光谱 DRS 与化学计量学相结合,可用于识别和量化中药材和食品的掺假行为。
{"title":"Detection of the Adulteration of Dendrobium Huoshanense with Dendrobium Henanense by UV-Vis-Shortwave Near-Infrared Diffuse Reflectance Spectroscopy Combined with Chemometrics.","authors":"Jing-Wen Hao, Nai-Dong Chen, Xiao-Quan Liu, Qiang Li, Hui-Min Xu, Wei-Han Yang, Chao-Feng Qin, Ya-Qing Bu","doi":"10.1093/jaoacint/qsad090","DOIUrl":"10.1093/jaoacint/qsad090","url":null,"abstract":"<p><strong>Background: </strong>Dendrobium huoshanense (DHS) is a classic traditional Chinese medicine (TCM) with distinctive medicinal benefits and great economic worth; nevertheless, because of similar tastes and looks, it is simple to adulterate with less expensive substitutes (such as Dendrobium henanense [DHN]).</p><p><strong>Objective: </strong>This work aimed to develop a reliable tool to detect and quantify the adulteration of DHS with DHN by using UV-Vis-shortwave near-infrared diffuse reflectance spectroscopy (UV-Vis-SWNIR DRS) combined with chemometrics.</p><p><strong>Methods: </strong>Adulterated samples prepared in varying concentrations (0-100%, w/w) were analyzed with UV-Vis-SWNIR DRS methods. Partial least-square-discriminant analysis (PLS-DA) and partial least-squares (PLS) regression techniques were used for the differentiation of adulterated DHN from pure DHS and the prediction of adulteration levels.</p><p><strong>Results: </strong>The PLS-DA classification models successfully differentiated adulterated and nonadulterated DHS with an over 100% correct classification rate. UV-Vis-SWNIR DRS data were also successfully used to predict adulteration levels with a high coefficient of determination for calibration (0.9924) and prediction (0.9906) models and low error values for calibration (3.863%) and prediction (5.067%).</p><p><strong>Conclusion: </strong>UV-Vis-SWNIR DRS, as a fast and environmentally friendly tool, has great potential for both the identification and quantification of adulteration practices involving herbal medicines and foods.</p><p><strong>Highlights: </strong>UV-Vis-SWNIR DRS combined with chemometrics can be applied to identify and quantify the adulteration of herbal medicines and foods.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"158-163"},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9981228","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
Understanding the Stress Testing Characteristics of Apixaban, Structural Elucidation of a Novel Degradation Impurity, and Stability-Indicating Method Development for Quantification of Related Substances. 了解阿哌沙班的压力测试特性、新型降解杂质的结构阐明以及相关物质定量的稳定性指示方法开发。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad106
Srikanth Reddy Surukonti, M S Surendrababu

Background: People who have non-valvular atrial fibrillation may benefit from taking a new oral anticoagulant called apixaban, which has recently been given the green light by the U.S. Food and Drug Administration. During stress testing, apixaban was found to have a high degree of degradability when subjected to both acidic and basic conditions, and one significant unknown impurity was observed in addition to the major known impurities.

Objective: Our aim is the isolation and characterization of degradation product observed in stress/forced degradation studies, and also the development of a single HPLC method that is both reliable and accurate for quantifying all 10 related impurities of apixaban.

Methods: Preparative HPLC was used to isolate the degradation product, and 1H NMR, 13C NMR, and MS were used to elucidate the structure of the product. Additionally, a single reverse-phase (RP) HPLC method was developed for quantification of all related impurities of apixaban.

Results: Based on the spectral characterization data, the identified unknown degradation impurity was found to be a pH-independent hydrolysis degradation impurity of apixaban. The developed method is specific, linear, accurate, robust, and rugged.

Conclusion: The isolated and characterized impurities were the same as those found during stress testing. The developed method has been validated for its intended purpose in accordance with the regulatory requirements that were outlined.

Highlights: The unknown impurity is a new apixaban degradation impurity that helps us understand its toxicity. The scientific community will benefit from the developed analytical method information as it relates to understanding drug product impurity profiling.

背景:非瓣膜性心房颤动患者可能会从服用一种名为阿哌沙班的新型口服抗凝剂中获益,美国食品和药物管理局最近为该药物开了绿灯。在压力测试中发现,阿哌沙班在酸性和碱性条件下都有很高的降解性,除了主要的已知杂质外,还发现了一种重要的未知杂质:我们的目的是分离和鉴定在应力/强制降解研究中观察到的降解产物,同时开发一种既可靠又准确的单一高效液相色谱法,用于定量阿哌沙班的所有 10 种相关杂质:方法:使用制备型高效液相色谱法分离降解产物,并使用 1H NMR、13C NMR 和 MS 来阐明产物的结构。此外,还开发了一种单一反相 (RP) 高效液相色谱法,用于定量分析阿哌沙班的所有相关杂质:结果:根据光谱表征数据,发现未知降解杂质是阿哌沙班的一种与pH值无关的水解降解杂质。所开发的方法特异、线性、准确、稳健、耐用:结论:分离和表征的杂质与应力测试中发现的杂质相同。结论:分离和表征的杂质与压力测试中发现的杂质相同,所开发的方法已根据概述的监管要求验证了其预期目的:未知杂质是一种新的阿哌沙班降解杂质,有助于我们了解阿哌沙班的毒性。科学界将从所开发的分析方法信息中获益,因为这关系到对药物产品杂质剖析的理解。
{"title":"Understanding the Stress Testing Characteristics of Apixaban, Structural Elucidation of a Novel Degradation Impurity, and Stability-Indicating Method Development for Quantification of Related Substances.","authors":"Srikanth Reddy Surukonti, M S Surendrababu","doi":"10.1093/jaoacint/qsad106","DOIUrl":"10.1093/jaoacint/qsad106","url":null,"abstract":"<p><strong>Background: </strong>People who have non-valvular atrial fibrillation may benefit from taking a new oral anticoagulant called apixaban, which has recently been given the green light by the U.S. Food and Drug Administration. During stress testing, apixaban was found to have a high degree of degradability when subjected to both acidic and basic conditions, and one significant unknown impurity was observed in addition to the major known impurities.</p><p><strong>Objective: </strong>Our aim is the isolation and characterization of degradation product observed in stress/forced degradation studies, and also the development of a single HPLC method that is both reliable and accurate for quantifying all 10 related impurities of apixaban.</p><p><strong>Methods: </strong>Preparative HPLC was used to isolate the degradation product, and 1H NMR, 13C NMR, and MS were used to elucidate the structure of the product. Additionally, a single reverse-phase (RP) HPLC method was developed for quantification of all related impurities of apixaban.</p><p><strong>Results: </strong>Based on the spectral characterization data, the identified unknown degradation impurity was found to be a pH-independent hydrolysis degradation impurity of apixaban. The developed method is specific, linear, accurate, robust, and rugged.</p><p><strong>Conclusion: </strong>The isolated and characterized impurities were the same as those found during stress testing. The developed method has been validated for its intended purpose in accordance with the regulatory requirements that were outlined.</p><p><strong>Highlights: </strong>The unknown impurity is a new apixaban degradation impurity that helps us understand its toxicity. The scientific community will benefit from the developed analytical method information as it relates to understanding drug product impurity profiling.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"22-30"},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10224104","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
A Green-and-White Integrative Analytical Strategy Combining Univariate and Chemometric Techniques for Quantifying Recently Approved Multi-Drug Eye Solution and Potentially Cancer-Causing Impurities: Application to the Aqueous Humor. 结合单变量和化学计量技术的绿白综合分析策略,用于定量最近批准的多种药物眼药水和潜在的致癌杂质:应用于水介质。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad087
Khalid A M Attia, Ahmed El-Olemy, Sherif M Eid, Ahmed Emad F Abbas

Background: Drug impurities are now seen as a major threat to the production of pharmaceuticals around the world and a major part of the global contamination problem, especially when it comes to carcinogenic impurities.

Objective: We present the first spectrophotometric strategy based on a combination of univariate and multivariate methods as impurity profiling methods for the estimation of lignocaine (LIG) and fluorescein (FLS) with their carcinogenic impurities: 2,6-xylidine (XYL) and benzene-1,3-diol (BZD).

Method: The data processing strategy depends on overcoming unresolved bands by employing five affordable, accurate, selective, and sensitive methods. The methods applied were a direct UV univariate spectrophotometric analysis (D0) and four multivariate chemometric methods, including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), and genetic algorithm (GA-PLS). FLS analysis (1-16 μg/mL) was performed using the D0 method at 478 nm; then, the application of the ratio subtraction method (RSM) allowed the removal of interference caused by the FLS spectrum. From the resulting ratio spectra, LIG, XYL, and BZD can be efficiently determined by chemometrics. The calibration set was carefully selected at five concentration levels using a partial factorial training design, resulting in 25 mixtures with central levels of 160, 40, and 3 μg/mL for LIG, XYL, and BZD, respectively. Another 13 samples were applied to validate the predictive ability.

Results: The statistical parameters demonstrated exceptional recoveries and smaller prediction errors, confirming the experimental model's predictive power.

Conclusions: The proposed approach was effectively tested using newly FDA-approved LIG and FLS pharmaceutical preparation and aqueous humor. Additionally, it was effectively assessed for whiteness, greenness, and sustainability using five assessment tools.

Highlights: With its remarkable analytical performance, sustainability, affordability, simplicity, and cost-efficiency, the proposed strategy is an indispensable tool for quality control and in situ analysis in little-equipped laboratories, increasing the proposed approach's surveillance ability.

背景:药物杂质现已被视为全球药品生产的主要威胁,也是全球污染问题的主要部分,尤其是致癌杂质:我们首次提出了基于单变量和多变量相结合的分光光度法杂质分析方法,用于估计木质素(LIG)和荧光素(FLS)及其致癌杂质:2,6-二甲基甲酰胺(XYL)和苯-1,3-二醇(BZD):数据处理策略取决于采用五种经济、准确、选择性强且灵敏的方法来克服未分辨带。采用的方法包括直接紫外单变量分光光度分析法(D0)和四种多元化学计量法,包括经典最小二乘法(CLS)、主成分回归法(PCR)、偏最小二乘法(PLS)和遗传算法(GA-PLS)。FLS 分析(1-16 μg/mL)是在 478 纳米波长下使用 D0 方法进行的;然后,应用比值减法(RSM)可以去除 FLS 光谱造成的干扰。根据得到的比值光谱,可以通过化学计量学有效地确定 LIG、XYL 和 BZD。通过部分因子训练设计,在五个浓度水平上仔细选择了校准集,最终得到了 25 种混合物,其 LIG、XYL 和 BZD 的中心浓度水平分别为 160、40 和 3 μg/mL。另外 13 个样本用于验证预测能力:统计参数显示了优异的回收率和较小的预测误差,证实了实验模型的预测能力:结论:利用新近获得 FDA 批准的 LIG 和 FLS 药物制剂以及水样,对所提出的方法进行了有效测试。结论:使用新近获得 FDA 批准的 LIG 和 FLS 药物制剂以及水溶液对所提出的方法进行了有效测试,并使用五种评估工具对其白度、绿色度和可持续性进行了有效评估:亮点:所提出的策略具有卓越的分析性能、可持续性、可负担性、简便性和成本效益,是设备简陋的实验室进行质量控制和现场分析不可或缺的工具,提高了所提出方法的监控能力。
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引用次数: 0
Fluoride Determination in Milk, Soy, and Water-Based Products Using Ion-Selective Electrode and Direct Measurement Technique: Single-Laboratory Validation, First Action 2022.05. 使用离子选择性电极和直接测量技术测定牛奶、大豆和水基产品中的氟化物:单实验室验证,首次行动 2022.05。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-04 DOI: 10.1093/jaoacint/qsad104
Renée M Erney, Charles K Black

Background: The AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals issued a call for methods for the determination of fluoride in infant formula. Standard Method Performance Requirement (SMPR®) 2014.016 was approved.

Objective: A single-laboratory validation (SLV) of a fluoride ion-selective electrode (F-ISE) method was completed.

Methods: Five powder samples were reconstituted, and hydrochloric acid was added to dissolve and release any bound fluoride. Samples included infant and adult nutritional products made from milk, whey, or soy, containing intact, partially hydrolyzed, or hydrolyzed proteins. Sodium citrate buffer was added to complex any interfering ions and adjust pH and ionic strength. Samples were analyzed in duplicate over 6 days using F-ISE.

Results: Results were calculated based on one of two least-squares (log fit) standard curves (0.02 to 0.1 µg/100 g or 0.1 to 2.0 µg/100 g). The LOQ for the method was determined to be 3.3 µg/100 g, which was far below the minimum analytical value of 30 µg/100 g required in the SMPR. The fluoride concentrations ranged from approximately 3 to 14 µg/100 g reconstituted powder and the intermediate precision, RSDr, ranged from 0.7 to 12.4%. Although all of these results are out of scope for the SMPR due to their low fluoride, it should be noted that the RSDr for formulas with fluoride concentrations ranging from approximately 9 to 14 µg/100 g ranged from 0.7 to 4.3%, and the RSDr for the two formulas with fluoride concentrations at or below the theoretical detection limit of the method were only approximately10 and 12.4%. Recoveries ranged from 94 to 98% for samples spiked at three levels with NIST-traceable standard solutions, meeting the SMPR.

Conclusion: The F-ISE method meets the SMPR and was adopted as a First Action Official MethodSM.

Highlights: The fluoride ion-selective electrode method presented here is affordable and easy to run. The addition of acid to the samples dissolves any minerals which may bind the fluoride.

背景:AOAC 婴儿配方奶粉和成人营养品利益相关者小组发布了一项关于婴儿配方奶粉中氟测定方法的征集令。标准方法性能要求 (SMPR®) 2014.016 获得批准:完成了氟离子选择电极 (F-ISE) 方法的单实验室验证 (SLV):方法: 对五份粉末样品进行重组,并加入盐酸溶解和释放结合的氟化物。样品包括由牛奶、乳清或大豆制成的婴幼儿和成人营养品,含有完整、部分水解或水解蛋白。加入柠檬酸钠缓冲液以络合任何干扰离子,并调节 pH 值和离子强度。使用 F-ISE 对样品进行为期 6 天的重复分析:根据两条最小二乘(对数拟合)标准曲线(0.02 至 0.1 µg/100 g 或 0.1 至 2.0 µg/100 g)中的一条计算结果。该方法的 LOQ 被确定为 3.3 µg/100 g,远远低于 SMPR 要求的 30 µg/100 g 的最低分析值。氟浓度范围约为 3 至 14 微克/100 克重组粉末,中间精度 RSDr 范围为 0.7 至 12.4%。尽管由于氟含量较低,所有这些结果都超出了 SMPR 的范围,但值得注意的是,氟浓度约为 9 至 14 µg/100 g 的配方的 RSDr 为 0.7% 至 4.3%,而氟浓度达到或低于方法理论检测限的两种配方的 RSDr 仅为 10% 和 12.4%。用 NIST 可追溯标准溶液对三个水平的样品进行添加,回收率在 94% 到 98% 之间,符合 SMPR 标准:结论:F-ISE 方法符合 SMPR 标准,并被采纳为第一行动正式方法(First Action Official MethodSM):本文介绍的氟离子选择电极法经济实惠,易于操作。在样品中加入酸可溶解任何可能与氟结合的矿物质。
{"title":"Fluoride Determination in Milk, Soy, and Water-Based Products Using Ion-Selective Electrode and Direct Measurement Technique: Single-Laboratory Validation, First Action 2022.05.","authors":"Renée M Erney, Charles K Black","doi":"10.1093/jaoacint/qsad104","DOIUrl":"10.1093/jaoacint/qsad104","url":null,"abstract":"<p><strong>Background: </strong>The AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals issued a call for methods for the determination of fluoride in infant formula. Standard Method Performance Requirement (SMPR®) 2014.016 was approved.</p><p><strong>Objective: </strong>A single-laboratory validation (SLV) of a fluoride ion-selective electrode (F-ISE) method was completed.</p><p><strong>Methods: </strong>Five powder samples were reconstituted, and hydrochloric acid was added to dissolve and release any bound fluoride. Samples included infant and adult nutritional products made from milk, whey, or soy, containing intact, partially hydrolyzed, or hydrolyzed proteins. Sodium citrate buffer was added to complex any interfering ions and adjust pH and ionic strength. Samples were analyzed in duplicate over 6 days using F-ISE.</p><p><strong>Results: </strong>Results were calculated based on one of two least-squares (log fit) standard curves (0.02 to 0.1 µg/100 g or 0.1 to 2.0 µg/100 g). The LOQ for the method was determined to be 3.3 µg/100 g, which was far below the minimum analytical value of 30 µg/100 g required in the SMPR. The fluoride concentrations ranged from approximately 3 to 14 µg/100 g reconstituted powder and the intermediate precision, RSDr, ranged from 0.7 to 12.4%. Although all of these results are out of scope for the SMPR due to their low fluoride, it should be noted that the RSDr for formulas with fluoride concentrations ranging from approximately 9 to 14 µg/100 g ranged from 0.7 to 4.3%, and the RSDr for the two formulas with fluoride concentrations at or below the theoretical detection limit of the method were only approximately10 and 12.4%. Recoveries ranged from 94 to 98% for samples spiked at three levels with NIST-traceable standard solutions, meeting the SMPR.</p><p><strong>Conclusion: </strong>The F-ISE method meets the SMPR and was adopted as a First Action Official MethodSM.</p><p><strong>Highlights: </strong>The fluoride ion-selective electrode method presented here is affordable and easy to run. The addition of acid to the samples dissolves any minerals which may bind the fluoride.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"103-111"},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10277601","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
期刊
Journal of AOAC International
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