首页 > 最新文献

Journal of AOAC International最新文献

英文 中文
Relevance of Secondary Enrichment in the Detection of Salmonella Spp in Food Samples by qPCR according to DIN 10135 根据 DIN 10135 标准通过 qPCR 检测食品样品中沙门氏菌属时二次富集的相关性
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2024-01-10 DOI: 10.1093/jaoacint/qsae002
F Codony, G Agustí, L Barreto, D Asensio
Background When detecting Salmonella spp. in food samples, unlike with culture-based procedures where there are solid standards, PCR techniques are generally dominated by commercial solutions, often backed by the conformity of reference organizations, and based on rigorous validation studies. The few independent standards that exist are not subject to revision and improvement to the same extent as the manufacturer's methods. Moreover, since commercial networks do not promote them, they are less implemented in everyday practice. The German standard DIN 10135 is an example of this. In this method, before PCR detection, a primary enrichment (16–20 h) followed by a secondary selective enrichment of at least 6 hours is needed. Nevertheless, it allows the possibility of only apply the first step if evidence of their correct operation is provided. Objective To evaluate how necessary is the secondary enrichment for DIN 10135 standard. Methods Short and complete enrichment steps were compared in the context of the evaluation of the limit of detection for 11 types of food. Additionally, a blind assay was performed with 75 food samples. Results The data show that a simple primary enrichment may be sufficient and that the second selective enrichment with the tested matrices would not be strictly essential. The blind study obtained a 98.6% of trueness and precision of 100%. Conclusions At least for the end consumer products, a secondary enrichment of 6 hours is not necessary for all the products tested. Highlights In the context of the DIN 10135 standard, the primary enrichment (16–20 h, 37 ± 1 °C) can be enough for detecting Salmonella spp.
背景 在检测食品样本中的沙门氏菌时,与有可靠标准的培养基程序不同,PCR 技术通常以商业解决方案为主,这些解决方案通常有参考组织的一致性支持,并以严格的验证研究为基础。现有的少数几个独立标准并不像制造商的方法那样需要修订和改进。此外,由于商业网络并不推广这些标准,它们在日常实践中的应用也较少。德国 DIN 10135 标准就是一个例子。在这种方法中,在 PCR 检测之前,需要先进行一次富集(16-20 小时),然后再进行至少 6 小时的二次选择性富集。不过,如果能提供正确操作的证据,也可以只进行第一步。目标 评估根据 DIN 10135 标准进行二次富集的必要性。方法 在对 11 种食品的检测限进行评估时,对短时间富集步骤和完全富集步骤进行比较。此外,还对 75 种食品样品进行了盲测。结果 数据显示,简单的初级富集可能就足够了,用被测基质进行第二次选择性富集并非绝对必要。盲法研究的真实度为 98.6%,精确度为 100%。结论 至少对于最终消费品来说,所有受测产品都没有必要进行 6 小时的二次富集。要点 根据 DIN 10135 标准,初级富集(16-20 小时,37 ± 1 °C)足以检测沙门氏菌属。
{"title":"Relevance of Secondary Enrichment in the Detection of Salmonella Spp in Food Samples by qPCR according to DIN 10135","authors":"F Codony, G Agustí, L Barreto, D Asensio","doi":"10.1093/jaoacint/qsae002","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae002","url":null,"abstract":"Background When detecting Salmonella spp. in food samples, unlike with culture-based procedures where there are solid standards, PCR techniques are generally dominated by commercial solutions, often backed by the conformity of reference organizations, and based on rigorous validation studies. The few independent standards that exist are not subject to revision and improvement to the same extent as the manufacturer's methods. Moreover, since commercial networks do not promote them, they are less implemented in everyday practice. The German standard DIN 10135 is an example of this. In this method, before PCR detection, a primary enrichment (16–20 h) followed by a secondary selective enrichment of at least 6 hours is needed. Nevertheless, it allows the possibility of only apply the first step if evidence of their correct operation is provided. Objective To evaluate how necessary is the secondary enrichment for DIN 10135 standard. Methods Short and complete enrichment steps were compared in the context of the evaluation of the limit of detection for 11 types of food. Additionally, a blind assay was performed with 75 food samples. Results The data show that a simple primary enrichment may be sufficient and that the second selective enrichment with the tested matrices would not be strictly essential. The blind study obtained a 98.6% of trueness and precision of 100%. Conclusions At least for the end consumer products, a secondary enrichment of 6 hours is not necessary for all the products tested. Highlights In the context of the DIN 10135 standard, the primary enrichment (16–20 h, 37 ± 1 °C) can be enough for detecting Salmonella spp.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462938","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
Stability Study Through Water Activity Measurements for Dispensed Powdered Raw Materials 通过测量配料粉末原料的水活性进行稳定性研究
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2024-01-09 DOI: 10.1093/jaoacint/qsae005
Harold A Prada-Ramírez, Juan Pablo Montes-Tamara, Eduardo A Rico-Jimenez, Juan Camilo Fonseca
Background Holding times for raw materials are relevant, since they enable us to understand the allowable time that a raw material can be kept under ideal storage conditions before the start of the manufacturing process without its quality attributes being affected. The quantification of water activity can be used as an indicator of the microbiological, physicochemical, and organoleptic stability of a specimen, since low water activity retards autohydrolysis and microbiological growth. Objective The main purpose of this investigation was to test the stability of powdered raw materials for a maximum holding time of 8 days through water activity measurements. Thus microbiological, physicochemical, and organoleptic measurements were carried out in parallel and simultaneously in order to experimentally establish a relationship between the status of the water activity of processed raw materials and the microbiological, physicochemical, and organoleptic results. Results The raw materials were stored for a maximum holding time of 8 days, in accordance with USP monographs. For all the raw materials tested, water activity measurements were performed using the dew point chilled-mirror method on days 0, 3, and 8. On days 0 and 8, microbiological, physicochemical, and organoleptic assessments were performed. It was established that under these storage conditions, the processed raw materials exhibited water activity below 0.60 during the entire holding time. However, there were statistically significant differences in water activity levels between days 0, 3, and 8 (ANOVA P < 0.05). Despite observing statistically significant differences between days, the microbiological, physicochemical, and organoleptic features were within specification at those water activity levels, below 0.60. Conclusion Water activity below 0.60 does not allow the growth of microorganisms, and the organoleptic and physicochemical features remain unperturbed. The results indicate that water activity can be used as an indicator of the microbiological load and chemical stability of the raw materials tested.
原材料的背景保持时间非常重要,因为它能让我们了解在生产过程开始前,原材料在理想的储存条件下可以保持多长时间而不会影响其质量属性。水活度的定量可作为试样的微生物、物理化学和感官稳定性的指标,因为低水活度可阻止自水解和微生物生长。本研究的主要目的是通过测量水活度来检测粉末状原材料在最长 8 天的保存时间内的稳定性。因此,微生物、物理化学和感官测量同时并行进行,以便通过实验确定加工原料的水活性状态与微生物、物理化学和感官结果之间的关系。结果 根据美国药典(USP)各专著的规定,原材料的最长保存时间为 8 天。在第 0 天、第 3 天和第 8 天,使用露点冷镜法对所有受测原料的水活性进行了测量。在第 0 天和第 8 天,进行了微生物、物理化学和感官评估。结果表明,在这些贮藏条件下,经过加工的原材料在整个贮藏期间的水分活度均低于 0.60。不过,在第 0、3 和 8 天之间,水活性水平存在显著的统计学差异(方差分析 P < 0.05)。尽管不同天数之间存在显著的统计学差异,但在水活度低于 0.60 的情况下,微生物、物理化学和感官特征均符合规范要求。结论 水活度低于 0.60 时,微生物无法生长,感官和理化特性也不会受到影响。结果表明,水活度可用作测试原材料微生物含量和化学稳定性的指标。
{"title":"Stability Study Through Water Activity Measurements for Dispensed Powdered Raw Materials","authors":"Harold A Prada-Ramírez, Juan Pablo Montes-Tamara, Eduardo A Rico-Jimenez, Juan Camilo Fonseca","doi":"10.1093/jaoacint/qsae005","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae005","url":null,"abstract":"Background Holding times for raw materials are relevant, since they enable us to understand the allowable time that a raw material can be kept under ideal storage conditions before the start of the manufacturing process without its quality attributes being affected. The quantification of water activity can be used as an indicator of the microbiological, physicochemical, and organoleptic stability of a specimen, since low water activity retards autohydrolysis and microbiological growth. Objective The main purpose of this investigation was to test the stability of powdered raw materials for a maximum holding time of 8 days through water activity measurements. Thus microbiological, physicochemical, and organoleptic measurements were carried out in parallel and simultaneously in order to experimentally establish a relationship between the status of the water activity of processed raw materials and the microbiological, physicochemical, and organoleptic results. Results The raw materials were stored for a maximum holding time of 8 days, in accordance with USP monographs. For all the raw materials tested, water activity measurements were performed using the dew point chilled-mirror method on days 0, 3, and 8. On days 0 and 8, microbiological, physicochemical, and organoleptic assessments were performed. It was established that under these storage conditions, the processed raw materials exhibited water activity below 0.60 during the entire holding time. However, there were statistically significant differences in water activity levels between days 0, 3, and 8 (ANOVA P < 0.05). Despite observing statistically significant differences between days, the microbiological, physicochemical, and organoleptic features were within specification at those water activity levels, below 0.60. Conclusion Water activity below 0.60 does not allow the growth of microorganisms, and the organoleptic and physicochemical features remain unperturbed. The results indicate that water activity can be used as an indicator of the microbiological load and chemical stability of the raw materials tested.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462985","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 Seven Human Milk Oligosaccharides (HMO) in Infant Formula and Adult Nutritionals: First Action 2022.07 测定婴儿配方奶粉和成人营养品中的七种母乳低聚糖 (HMO):首次行动 2022.07
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2024-01-09 DOI: 10.1093/jaoacint/qsae001
Thierry Bénet, Nathalie Frei, Véronique Spichtig, Denis Cuany, Sean Austin
Background Human milk oligosaccharides (HMOs) are important components of breast milk and may be responsible for some of the benefits of breastfeeding, including resistance to infections and the development of a healthy gut microbiota. Selected HMOs are now available for addition to infant formula, and suitable methods to control the dosing rate are needed. Objective To develop and validate a suitable method for the analysis of HMOs in infant formula. Method A method was developed for the determination of seven human milk oligosaccharides (2’-fucosyllactose, 3-fucosyllactose, 3’-sialyllactose, 6’-sialyllactose (6’SL), 2’,3-difucosyllactose, lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT)) in infant formula and adult nutritionals. The oligosaccharides are labelled at their reducing end with 2-aminobenzamide, separated by liquid chromatography and detected using a fluorescence detector. Maltodextrins are enzymatically hydrolyzed before analysis to prevent potential interference, likewise an optional β-galactosidase treatment can be used to remove β-galactooligosaccharides. Fructooligosaccharides or polydextrose do not generally interfere with the analysis. Results The method has been validated in a single laboratory on infant formula and adult nutritionals. The seven HMOs were spiked in to eight matrices at three or four spike levels giving a total of 176 data points. Recoveries were in the range 90.9–109% in all cases except at the lowest spike level in one matrix (elemental formula), where the LNT recovery was 113%, the LNnT recovery was 111% and the 6’SL recovery was 121%. Relative repeatabilities (RSD(r)) were in the range 0.1–4.2%. The performance is generally within the requirements outlined in the Standard Method Performance Requirements (SMPR®) published by AOAC International. Conclusions The method developed is suitable for the determination of seven HMOs in infant formula and demonstrated good performance during single laboratory validation. Highlights A method has been developed which is suitable for the determination of seven HMOs in infant formula.
背景 母乳低聚糖(HMOs)是母乳的重要成分,可能是母乳喂养的一些益处,包括抗感染和健康肠道微生物群的发育。目前,部分 HMO 可添加到婴儿配方奶粉中,但需要合适的方法来控制添加量。目标 开发并验证分析婴儿配方奶粉中 HMOs 的合适方法。方法 建立了一种测定婴儿配方奶粉和成人营养品中七种人乳低聚糖(2'-岩藻酰乳糖、3-岩藻酰乳糖、3'-硅藻酰乳糖、6'-硅藻酰乳糖(6'SL)、2',3-二岩藻酰乳糖、乳-N-四糖(LNT)、乳-N-新四糖(LNnT))的方法。低聚糖的还原端用 2- 氨基苯甲酰胺标记,用液相色谱法分离,并用荧光检测器检测。麦芽糊精在分析前会被酶水解,以防止潜在的干扰,同样,β-半乳糖苷酶处理也可用于去除β-半乳寡糖。果寡糖或聚葡萄糖一般不会干扰分析。结果 该方法已在一家实验室对婴儿配方奶粉和成人营养品进行了验证。在八种基质中添加了三种或四种 HMO,共得到 176 个数据点。除一种基质(元素配方)中最低加标水平的 LNT 回收率为 113%、LNnT 回收率为 111%、6'SL 回收率为 121%外,所有情况下的回收率都在 90.9-109% 之间。相对重复性 (RSD(r)) 在 0.1-4.2% 之间。其性能基本符合 AOAC 国际公布的《标准方法性能要求》(SMPR®)中列出的要求。结论 所开发的方法适用于测定婴儿配方奶粉中的七种 HMOs,并在单一实验室验证过程中表现出良好的性能。要点 已开发出一种适用于测定婴儿配方奶粉中七种 HMOs 的方法。
{"title":"Determination of Seven Human Milk Oligosaccharides (HMO) in Infant Formula and Adult Nutritionals: First Action 2022.07","authors":"Thierry Bénet, Nathalie Frei, Véronique Spichtig, Denis Cuany, Sean Austin","doi":"10.1093/jaoacint/qsae001","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae001","url":null,"abstract":"Background Human milk oligosaccharides (HMOs) are important components of breast milk and may be responsible for some of the benefits of breastfeeding, including resistance to infections and the development of a healthy gut microbiota. Selected HMOs are now available for addition to infant formula, and suitable methods to control the dosing rate are needed. Objective To develop and validate a suitable method for the analysis of HMOs in infant formula. Method A method was developed for the determination of seven human milk oligosaccharides (2’-fucosyllactose, 3-fucosyllactose, 3’-sialyllactose, 6’-sialyllactose (6’SL), 2’,3-difucosyllactose, lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT)) in infant formula and adult nutritionals. The oligosaccharides are labelled at their reducing end with 2-aminobenzamide, separated by liquid chromatography and detected using a fluorescence detector. Maltodextrins are enzymatically hydrolyzed before analysis to prevent potential interference, likewise an optional β-galactosidase treatment can be used to remove β-galactooligosaccharides. Fructooligosaccharides or polydextrose do not generally interfere with the analysis. Results The method has been validated in a single laboratory on infant formula and adult nutritionals. The seven HMOs were spiked in to eight matrices at three or four spike levels giving a total of 176 data points. Recoveries were in the range 90.9–109% in all cases except at the lowest spike level in one matrix (elemental formula), where the LNT recovery was 113%, the LNnT recovery was 111% and the 6’SL recovery was 121%. Relative repeatabilities (RSD(r)) were in the range 0.1–4.2%. The performance is generally within the requirements outlined in the Standard Method Performance Requirements (SMPR®) published by AOAC International. Conclusions The method developed is suitable for the determination of seven HMOs in infant formula and demonstrated good performance during single laboratory validation. Highlights A method has been developed which is suitable for the determination of seven HMOs in infant formula.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462850","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
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 Q2 Medicine 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。
{"title":"Stability and Biosimilarity Assessment of Bevacizumab Monoclonal Antibody; Orthogonal Testing Protocol Coupled With Peptide Mapping-Principal Component Analysis.","authors":"Sara H Abdelghaffar, Maha A Hegazy, Basma M Eltanany","doi":"10.1093/jaoacint/qsad094","DOIUrl":"10.1093/jaoacint/qsad094","url":null,"abstract":"<p><strong>Background: </strong>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.</p><p><strong>Objective: </strong>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).</p><p><strong>Methods: </strong>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.</p><p><strong>Conclusions: </strong>The results obtained highlighted the importance of assessing similarities and differences in ensuring the biosimilarity and interchangeability of the studied products.</p><p><strong>Highlights: </strong>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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10414985","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
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 Q2 Medicine 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。
{"title":"Green HPLC Method for Simultaneous Analysis of Three Natural Antioxidants by Analytical Quality by Design.","authors":"Ramya Jonnalagadda, Seetharaman Rathinam, Krishnaveni Nagappan, Vinodhini Chandrasekar","doi":"10.1093/jaoacint/qsad105","DOIUrl":"10.1093/jaoacint/qsad105","url":null,"abstract":"<p><strong>Background: </strong>Glutathione, silybin, and curcumin are well-known potential antioxidants that are recommended as adjuvant therapy in cancer treatment.</p><p><strong>Objective: </strong>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.</p><p><strong>Method: </strong>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.</p><p><strong>Results: </strong>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.</p><p><strong>Conclusions: </strong>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.</p><p><strong>Highlights: </strong>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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10214818","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
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 Q2 Medicine 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。
{"title":"Smart Multivariate Spectrophotometric Determination of Two Co-Administered Autoimmune Drugs; Sulfasalazine and Pentoxifylline; in Bulk and Spiked Human Plasma.","authors":"Maimana A Magdy, Nehal F Farid, Basma H Anwar, Nessreen S Abdelhamid","doi":"10.1093/jaoacint/qsad097","DOIUrl":"10.1093/jaoacint/qsad097","url":null,"abstract":"<p><strong>Background: </strong>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.</p><p><strong>Objective: </strong>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.</p><p><strong>Methods: </strong>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.</p><p><strong>Results: </strong>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.</p><p><strong>Conclusion: </strong>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.</p><p><strong>Highlights: </strong>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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10052760","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 Q2 Medicine 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。
{"title":"Simultaneous Chromatographic Estimation of Vildagliptin and Dapagliflozin Using Hybrid Principles of White Analytical Chemistry and Analytical Quality by Design.","authors":"Pintu Prajapati, Bageshree Rana, Veera Shakar Pulusu, Shailesh Shah","doi":"10.1093/jaoacint/qsad108","DOIUrl":"10.1093/jaoacint/qsad108","url":null,"abstract":"<p><strong>Background: </strong>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.</p><p><strong>Objective: </strong>Hence, the WAC-based RP-HPLC method has been developed for the estimation of VDG and DGZ using lower toxic and economical solvents.</p><p><strong>Method: </strong>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.</p><p><strong>Results: </strong>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.</p><p><strong>Conclusions: </strong>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.</p><p><strong>Highlights: </strong>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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10277600","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 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 Q2 Medicine 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":null,"pages":null},"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
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 Q2 Medicine 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。
{"title":"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.","authors":"Nagavardhana Reddy Vanga, Venkata Ratnam Kesamsetty, Kumaraswamy Ummiti, Venkata Nadh Ratnakaram, Hanimi Reddy Bapatu","doi":"10.1093/jaoacint/qsad101","DOIUrl":"10.1093/jaoacint/qsad101","url":null,"abstract":"<p><strong>Background: </strong>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.</p><p><strong>Objective: </strong>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).</p><p><strong>Methods: </strong>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.</p><p><strong>Results: </strong>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%).</p><p><strong>Conclusion: </strong>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.</p><p><strong>Highlights: </strong>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.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2024-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10172141","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
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 Q2 Medicine 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":null,"pages":null},"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
期刊
Journal of AOAC International
全部 Acc. Chem. Res. ACS Applied Bio Materials ACS Appl. Electron. Mater. ACS Appl. Energy Mater. ACS Appl. Mater. Interfaces ACS Appl. Nano Mater. ACS Appl. Polym. Mater. ACS BIOMATER-SCI ENG ACS Catal. ACS Cent. Sci. ACS Chem. Biol. ACS Chemical Health & Safety ACS Chem. Neurosci. ACS Comb. Sci. ACS Earth Space Chem. ACS Energy Lett. ACS Infect. Dis. ACS Macro Lett. ACS Mater. Lett. ACS Med. Chem. Lett. ACS Nano ACS Omega ACS Photonics ACS Sens. ACS Sustainable Chem. Eng. ACS Synth. Biol. Anal. Chem. BIOCHEMISTRY-US Bioconjugate Chem. BIOMACROMOLECULES Chem. Res. Toxicol. Chem. Rev. Chem. Mater. CRYST GROWTH DES ENERG FUEL Environ. Sci. Technol. Environ. Sci. Technol. Lett. Eur. J. Inorg. Chem. IND ENG CHEM RES Inorg. Chem. J. Agric. Food. Chem. J. Chem. Eng. Data J. Chem. Educ. J. Chem. Inf. Model. J. Chem. Theory Comput. J. Med. Chem. J. Nat. Prod. J PROTEOME RES J. Am. Chem. Soc. LANGMUIR MACROMOLECULES Mol. Pharmaceutics Nano Lett. Org. Lett. ORG PROCESS RES DEV ORGANOMETALLICS J. Org. Chem. J. Phys. Chem. J. Phys. Chem. A J. Phys. Chem. B J. Phys. Chem. C J. Phys. Chem. Lett. Analyst Anal. Methods Biomater. Sci. Catal. Sci. Technol. Chem. Commun. Chem. Soc. Rev. CHEM EDUC RES PRACT CRYSTENGCOMM Dalton Trans. Energy Environ. Sci. ENVIRON SCI-NANO ENVIRON SCI-PROC IMP ENVIRON SCI-WAT RES Faraday Discuss. Food Funct. Green Chem. Inorg. Chem. Front. Integr. Biol. J. Anal. At. Spectrom. J. Mater. Chem. A J. Mater. Chem. B J. Mater. Chem. C Lab Chip Mater. Chem. Front. Mater. Horiz. MEDCHEMCOMM Metallomics Mol. Biosyst. Mol. Syst. Des. Eng. Nanoscale Nanoscale Horiz. Nat. Prod. Rep. New J. Chem. Org. Biomol. Chem. Org. Chem. Front. PHOTOCH PHOTOBIO SCI PCCP Polym. Chem.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1