Talanta Open最新文献_第2页

Trace-level quantification of NDMA in levosulpuride active pharmaceutical ingredient and tablet formulation Using UFLC-MS/MS 使用 UFLC-MS/MS 在左旋舒必利活性药物成分和片剂中痕量定量 NDMA

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-11-03 DOI: 10.1016/j.talo.2024.100375

Hemanth Vikram P․R , Gunjan Kumar , Rajashree Deka , Umme Hani , Nazima Haider , Sirajunisa Talath , Adil Farooq Wali , Dilipkumar Reddy Kandula , Narasimha M. Beeraka , Sinchana B Gopalaiah , Devi Sri Chiriki , Namitha Bannimath , Pramod Kumar , Bannimath Gurupadayya

Nitrosamine impurities identified in several pharmaceuticals during recent times has raised concerns leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated a ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of NDMA in Levosulpuride drug substance and tablet formulation. Current method utilizes a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Gemini NX-C18 column (150 × 4.6 mm, 3 µm) maintained at 40 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (methanol), with a total run time of 18 minutes. Current method achieved excellent linearity, recovery, precision, and sensitivity. Greenness of the developed method was evaluated using the GAPI, AGREE, and AES metrics. Current method is sensitive and selective for NDMA in levosulpuride drug substance and tablet formulations and can be employed for routine quality control analysis in pharmaceutical industry.

近来，在一些药品中发现的亚硝胺杂质引起了人们的关注，导致了全球范围内的产品召回，因此有必要采用灵敏的液相和气相色谱法对亚硝胺杂质进行痕量检测。本研究开发并验证了一种超快速液相色谱-串联质谱（UFLC-MS/MS）方法，用于定量检测左旋舒必利（Levosulpuride）药物和片剂中的 NDMA。该方法采用三重四极杆分析仪、常压化学电离（APCI）电离源和多反应监测（MRM）扫描模式进行分析。色谱分离采用 Gemini NX-C18 色谱柱（150 × 4.6 毫米，3 微米），色谱柱温度保持在 40 °C。流动相包括溶剂 A（0.1% 甲酸水溶液）和溶剂 B（甲醇）的二元梯度，总运行时间为 18 分钟。该方法在线性、回收率、精密度和灵敏度方面均表现优异。使用 GAPI、AGREE 和 AES 指标对所开发方法的绿色性进行了评估。本方法对左旋舒必利药物和片剂中的 NDMA 具有良好的灵敏度和选择性，可用于制药行业的常规质量控制分析。

{"title":"Trace-level quantification of NDMA in levosulpuride active pharmaceutical ingredient and tablet formulation Using UFLC-MS/MS","authors":"Hemanth Vikram P․R , Gunjan Kumar , Rajashree Deka , Umme Hani , Nazima Haider , Sirajunisa Talath , Adil Farooq Wali , Dilipkumar Reddy Kandula , Narasimha M. Beeraka , Sinchana B Gopalaiah , Devi Sri Chiriki , Namitha Bannimath , Pramod Kumar , Bannimath Gurupadayya","doi":"10.1016/j.talo.2024.100375","DOIUrl":"10.1016/j.talo.2024.100375","url":null,"abstract":"<div><div>Nitrosamine impurities identified in several pharmaceuticals during recent times has raised concerns leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated a ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of NDMA in Levosulpuride drug substance and tablet formulation. Current method utilizes a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Gemini NX-C18 column (150 × 4.6 mm, 3 µm) maintained at 40 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (methanol), with a total run time of 18 minutes. Current method achieved excellent linearity, recovery, precision, and sensitivity. Greenness of the developed method was evaluated using the GAPI, AGREE, and AES metrics. Current method is sensitive and selective for NDMA in levosulpuride drug substance and tablet formulations and can be employed for routine quality control analysis in pharmaceutical industry.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100375"},"PeriodicalIF":4.1,"publicationDate":"2024-11-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592729","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Development of nanomaterial-supported molecularly imprinted polymer/receptor-like sensor for the detection of rosuvastatin from binary mixtures 开发纳米材料支撑的分子印迹聚合物/受体样传感器，用于检测二元混合物中的罗伐他汀

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-11-03 DOI: 10.1016/j.talo.2024.100376

Mahdi Gharibi , Ensar Piskin , Nadia Bounoua , Ahmet Cetinkaya , Sibel A. Ozkan

Statins reduce cholesterol synthesis by inhibiting the enzyme hydroxymethylglutaryl-CoA (HMG-CoA) reductase. Rosuvastatin (ROS) is a statin drug used to prevent cardiovascular diseases and treat abnormal lipids. This study describes the design and fabrication of a nanomaterial-assisted molecularly imprinted polymer (MIP)-based electrochemical sensor for ROS determination. In addition, MIP-based electrochemical sensors were designed to detect ROS in both standard solutions and serum samples. In the MIP-based electrochemical sensor developed via the photopolymerization (PP) technique on the glassy carbon electrode (GCE) surface, were used zinc oxide nanoparticles (ZnO NPs) as a pore former, p-aminobenzoic acid (p-ABA) as functional monomer, ROS as template molecule. Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM) techniques were used to carry out detailed characterizations concerning surface morphology and electrochemistry. Under optimized experimental conditions, the linearity range of the designed sensor was found 1.0 × 10⁻¹³–1.0 × 10⁻¹² M. The superior selectivity of the MIP-based sensor against ROS in the presence of their binary mixtures was confirmed by interference studies. The recovery rates of the MIP-based sensors were calculated as 100.35 % and 99.16 % in commercial tablet form and serum samples, respectively. Moreover, the proposed sensor's relative selectivity coefficient (k′) was calculated, and it provided good selectivity for ROS over the NIP sensor. In conclusion, this newly developed sensor offers an advantageous approach for selective, sensitive, rapid and cost-effective analysis of ROS from binary mixtures. Additionally, this study is the first electrochemical sensor using nanomaterial-assisted MIP technology for ROS analysis, and its sensitivity is higher than that of other studies in the literature.

他汀类药物通过抑制羟甲基戊二酰-CoA（HMG-CoA）还原酶来减少胆固醇的合成。瑞舒伐他汀（ROS）是一种他汀类药物，用于预防心血管疾病和治疗血脂异常。本研究介绍了一种基于纳米材料辅助的分子印迹聚合物（MIP）电化学传感器的设计和制造，用于测定 ROS。此外，还设计了基于 MIP 的电化学传感器来检测标准溶液和血清样品中的 ROS。在玻璃碳电极（GCE）表面通过光聚合（PP）技术开发的基于 MIP 的电化学传感器中，使用氧化锌纳米颗粒（ZnO NPs）作为孔隙形成剂，对氨基苯甲酸（p-ABA）作为功能单体，ROS 作为模板分子。实验采用了电化学阻抗谱（EIS）、循环伏安法（CV）和扫描电子显微镜（SEM）技术，对表面形貌和电化学特性进行了详细分析。在优化的实验条件下，所设计传感器的线性范围为 1.0 × 10-13-1.0 × 10-12 M。根据计算，基于 MIP 的传感器在商业片剂和血清样品中的回收率分别为 100.35 % 和 99.16 %。此外，还计算了拟议传感器的相对选择性系数（k′），与 NIP 传感器相比，该传感器对 ROS 具有良好的选择性。总之，这种新开发的传感器为选择性、灵敏、快速和经济高效地分析二元混合物中的 ROS 提供了一种有利的方法。此外，该研究是首个使用纳米材料辅助 MIP 技术进行 ROS 分析的电化学传感器，其灵敏度高于其他文献研究。

{"title":"Development of nanomaterial-supported molecularly imprinted polymer/receptor-like sensor for the detection of rosuvastatin from binary mixtures","authors":"Mahdi Gharibi , Ensar Piskin , Nadia Bounoua , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.talo.2024.100376","DOIUrl":"10.1016/j.talo.2024.100376","url":null,"abstract":"<div><div>Statins reduce cholesterol synthesis by inhibiting the enzyme hydroxymethylglutaryl-CoA (HMG-CoA) reductase. Rosuvastatin (ROS) is a statin drug used to prevent cardiovascular diseases and treat abnormal lipids. This study describes the design and fabrication of a nanomaterial-assisted molecularly imprinted polymer (MIP)-based electrochemical sensor for ROS determination. In addition, MIP-based electrochemical sensors were designed to detect ROS in both standard solutions and serum samples. In the MIP-based electrochemical sensor developed via the photopolymerization (PP) technique on the glassy carbon electrode (GCE) surface, were used zinc oxide nanoparticles (ZnO NPs) as a pore former, p-aminobenzoic acid (p-ABA) as functional monomer, ROS as template molecule. Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM) techniques were used to carry out detailed characterizations concerning surface morphology and electrochemistry. Under optimized experimental conditions, the linearity range of the designed sensor was found 1.0 × 10<sup>−13</sup>–1.0 × 10<sup>−12</sup> M. The superior selectivity of the MIP-based sensor against ROS in the presence of their binary mixtures was confirmed by interference studies. The recovery rates of the MIP-based sensors were calculated as 100.35 % and 99.16 % in commercial tablet form and serum samples, respectively. Moreover, the proposed sensor's relative selectivity coefficient (k′) was calculated, and it provided good selectivity for ROS over the NIP sensor. In conclusion, this newly developed sensor offers an advantageous approach for selective, sensitive, rapid and cost-effective analysis of ROS from binary mixtures. Additionally, this study is the first electrochemical sensor using nanomaterial-assisted MIP technology for ROS analysis, and its sensitivity is higher than that of other studies in the literature.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100376"},"PeriodicalIF":4.1,"publicationDate":"2024-11-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592728","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Metal organic frameworks for bacterial detection in environmental samples 用于环境样本中细菌检测的金属有机框架

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-11-01 DOI: 10.1016/j.talo.2024.100374

Hadeer M. Bedair , Alaa Bedair , Mahmoud Hamed , Marcello Locatelli , Fotouh R. Mansour

Pathogenic bacteria pose significant threats to public health. Early and accurate detection of bacteria is crucial for infection control and prevention of outbreaks. This paper reviews recent advances in metal organic framework (MOF)-based methods for bacterial detection. MOFs are promising materials for biosensing due to their large surface areas, customizable properties, and ability to integrate various sensing capabilities. Several colorimetric and electrochemical detection techniques that utilize MOFs are discussed. Colorimetric assays combining MOFs with gold nanoparticles, peroxidase-mimicking activity, and aptamer recognition have achieved sensitive and specific detection of bacteria such as E. coli and S. aureus. Electrochemical biosensors integrating MOFs, antibodies, aptamers and quantum dots have also demonstrated low detection limits for various bacteria. Notably, techniques using MOF peroxidase-like activity coupled with magnetic separation or competitive binding assays show potential for point-of-care pathogen detection. Furthermore, optimization of MOF properties and integration within microfluidic platforms may lead to portable, low-cost and rapid methods suitable for on-site bacterial analysis in diverse settings. Continued exploration of MOF-based sensing strategies holds promise for improved bacteria monitoring and control of infectious diseases.

致病细菌对公共卫生构成重大威胁。及早准确地检测细菌对于控制感染和预防疫情爆发至关重要。本文回顾了基于金属有机框架（MOF）的细菌检测方法的最新进展。MOF 具有大表面积、可定制的特性以及整合各种传感功能的能力，因此是很有前景的生物传感材料。本文讨论了几种利用 MOFs 的比色和电化学检测技术。将 MOFs 与金纳米粒子、过氧化物酶模拟活性和适配体识别相结合的比色检测技术实现了对大肠杆菌和金黄色葡萄球菌等细菌的灵敏而特异的检测。集成了 MOFs、抗体、适配体和量子点的电化学生物传感器也证明了对各种细菌的低检测限。值得注意的是，利用 MOF 过氧化物酶样活性与磁分离或竞争性结合检测相结合的技术显示出了用于护理点病原体检测的潜力。此外，优化 MOF 的特性并将其集成到微流控平台中，可能会产生便携式、低成本和快速的方法，适用于各种环境下的现场细菌分析。继续探索基于 MOF 的传感策略有望改善细菌监测和传染病控制。

{"title":"Metal organic frameworks for bacterial detection in environmental samples","authors":"Hadeer M. Bedair , Alaa Bedair , Mahmoud Hamed , Marcello Locatelli , Fotouh R. Mansour","doi":"10.1016/j.talo.2024.100374","DOIUrl":"10.1016/j.talo.2024.100374","url":null,"abstract":"<div><div>Pathogenic bacteria pose significant threats to public health. Early and accurate detection of bacteria is crucial for infection control and prevention of outbreaks. This paper reviews recent advances in metal organic framework (MOF)-based methods for bacterial detection. MOFs are promising materials for biosensing due to their large surface areas, customizable properties, and ability to integrate various sensing capabilities. Several colorimetric and electrochemical detection techniques that utilize MOFs are discussed. Colorimetric assays combining MOFs with gold nanoparticles, peroxidase-mimicking activity, and aptamer recognition have achieved sensitive and specific detection of bacteria such as <em>E. coli</em> and <em>S. aureus</em>. Electrochemical biosensors integrating MOFs, antibodies, aptamers and quantum dots have also demonstrated low detection limits for various bacteria. Notably, techniques using MOF peroxidase-like activity coupled with magnetic separation or competitive binding assays show potential for point-of-care pathogen detection. Furthermore, optimization of MOF properties and integration within microfluidic platforms may lead to portable, low-cost and rapid methods suitable for on-site bacterial analysis in diverse settings. Continued exploration of MOF-based sensing strategies holds promise for improved bacteria monitoring and control of infectious diseases.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100374"},"PeriodicalIF":4.1,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142662612","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Accurate low-dose exposure assessment of benzene and monoaromatic compounds by diffusive sampling: Sampling and analytical method validation according to ISO 23320 for radiello® samplers packed with graphitised charcoal and suitable for thermal desorption 通过扩散采样对苯和单芳香族化合物进行精确的低剂量暴露评估：根据 ISO 23320 标准对装有石墨化木炭并适合热脱附的 radiello® 采样器进行采样和分析方法验证

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-30 DOI: 10.1016/j.talo.2024.100372

Laura Zaratin , Caterina Boaretto , Riccardo Carnevale Schianca , George Hinkal , Elena Grignani , Danilo Cottica

This research was aimed at providing an accurate low-dose benzene exposure assessment method, prospectively suitable to exposure limit values in the low ppb range, such as in the present-day chemical, petrochemical, foundry and pharmaceutical industry. The project addresses the need for a robust and fully validated method of personal exposure measurements considering that the Occupational Exposure Limit Value for benzene will be significantly lowered in the next few years. Diffusive sampling offers a reliable alternative to pumped sampling methods, intrinsic safety in potentially explosive atmospheres, lightness and ease of use. The tested diffusive sampler is radiello® with the RAD145 adsorption substrate. This configuration is packed with graphitised charcoal suitable for thermal desorption and analysis by HRGC-FID or HRGC-MS.

The experiments have been conducted following the ISO 23320 standard in the range from 0.005 to 0.1 ppm (16 to 320 µg/m³), yielding a full validation of the sampling and analytical method. The sampler performances have fulfilled all requisites of the ISO 23320 standard, in particular: bias due to the selection of a non-ideal sorbent is lower than 10 % (no significant back diffusion of benzene due to concentration change in the atmosphere); bias due to storage of samples for up to 2 months is lower than 10 %; nominal uptake rate for benzene on RAD145 is 32.3 mL/min; expanded uncertainty of the sampling and analytical method is 22.1 % in the concentration range from 80 to 320 µg/m³. The sampling and analytical method is therefore fit-for-purpose for the personal exposure measurements aimed at testing compliance with lowered occupational exposure limit values for benzene. The method is also fit for short duration exposure monitoring related to specific tasks, and other volatile organic compounds, usually found in the same workplaces, such as aliphatic and aromatic hydrocarbons and some oxygenated compounds, have been also studied. In particular, n-hexane and isopropyl benzene (also known as cumene), whose classification is currently under revision, can be efficiently monitored by this technique.

这项研究旨在提供一种准确的低剂量苯暴露评估方法，该方法有望适用于低 ppb 范围内的暴露限值，例如当今的化工、石化、铸造和制药行业。考虑到苯的职业接触限值将在未来几年内大幅降低，该项目需要一种可靠且经过充分验证的个人接触测量方法。扩散采样法是泵送采样法的可靠替代方法，在潜在爆炸性气体环境中具有内在安全性、轻便性和易用性。经过测试的扩散采样器是带有 RAD145 吸附基板的 radiello®。实验按照 ISO 23320 标准在 0.005 至 0.1 ppm（16 至 320 µg/m3）范围内进行，对采样和分析方法进行了全面验证。采样器的性能符合 ISO 23320 标准的所有要求，特别是：选择非理想吸附剂造成的偏差低于 10%（大气中的浓度变化不会导致苯的明显反向扩散）；样品储存长达 2 个月造成的偏差低于 10%；RAD145 对苯的标称吸收率为 32.3 mL/min；在 80 至 320 µg/m³ 的浓度范围内，采样和分析方法的扩展不确定度为 22.1%。因此，该采样和分析方法适用于个人接触测量，旨在检测是否符合降低后的苯职业接触限值。该方法也适用于与特定任务相关的短时间暴露监测，而且还研究了通常在同一工作场所发现的其他挥发性有机化合物，如脂肪族和芳香族碳氢化合物以及一些含氧化合物。特别是，正己烷和异丙苯（又称 "积苯"），其分类目前正在修订中，可以通过这种技术进行有效监测。

{"title":"Accurate low-dose exposure assessment of benzene and monoaromatic compounds by diffusive sampling: Sampling and analytical method validation according to ISO 23320 for radiello® samplers packed with graphitised charcoal and suitable for thermal desorption","authors":"Laura Zaratin , Caterina Boaretto , Riccardo Carnevale Schianca , George Hinkal , Elena Grignani , Danilo Cottica","doi":"10.1016/j.talo.2024.100372","DOIUrl":"10.1016/j.talo.2024.100372","url":null,"abstract":"<div><div>This research was aimed at providing an accurate low-dose benzene exposure assessment method, prospectively suitable to exposure limit values in the low ppb range, such as in the present-day chemical, petrochemical, foundry and pharmaceutical industry. The project addresses the need for a robust and fully validated method of personal exposure measurements considering that the Occupational Exposure Limit Value for benzene will be significantly lowered in the next few years. Diffusive sampling offers a reliable alternative to pumped sampling methods, intrinsic safety in potentially explosive atmospheres, lightness and ease of use. The tested diffusive sampler is <em>radiello</em>® with the RAD145 adsorption substrate. This configuration is packed with graphitised charcoal suitable for thermal desorption and analysis by HRGC-FID or HRGC-MS.</div><div>The experiments have been conducted following the ISO 23320 standard in the range from 0.005 to 0.1 ppm (16 to 320 µg/m<sup>3</sup>), yielding a full validation of the sampling and analytical method. The sampler performances have fulfilled all requisites of the ISO 23320 standard, in particular: bias due to the selection of a non-ideal sorbent is lower than 10 % (no significant back diffusion of benzene due to concentration change in the atmosphere); bias due to storage of samples for up to 2 months is lower than 10 %; nominal uptake rate for benzene on RAD145 is 32.3 mL/min; expanded uncertainty of the sampling and analytical method is 22.1 % in the concentration range from 80 to 320 µg/m³. The sampling and analytical method is therefore fit-for-purpose for the personal exposure measurements aimed at testing compliance with lowered occupational exposure limit values for benzene. The method is also fit for short duration exposure monitoring related to specific tasks, and other volatile organic compounds, usually found in the same workplaces, such as aliphatic and aromatic hydrocarbons and some oxygenated compounds, have been also studied. In particular, n-hexane and isopropyl benzene (also known as cumene), whose classification is currently under revision, can be efficiently monitored by this technique.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100372"},"PeriodicalIF":4.1,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592730","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Advancing electrochemical sensing: A smart platform for accurate CRP level detection in neonatal septicaemia 推进电化学传感技术：用于准确检测新生儿败血症 CRP 水平的智能平台

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-18 DOI: 10.1016/j.talo.2024.100369

Sapna Balayan , Nidhi Chauhan , Vinita Hooda , Ramesh Chandra , Warren Rosario , Utkarsh Jain

Neonatal septicaemia is an intricate systemic affliction induced in newborns. A multitude of fungi, viruses, and bacteria elicit this condition. Conventional methodologies such as radiological imaging, microbial testing, blood culture, and inflammatory markers suffer from an array of constraints for prompt detection of infection. This present study illustrates a cutting-edge smart electrochemical biosensing system. The fabricated system was meticulously engineered to discern the concentration of C-reactive protein (CRP). CRP is an irreplaceable prognostic indicator for neonatal sepsis. This work explicates the fabrication of a bioreceptor sensing platform (BioRe Sense) on a screen-printed miniaturized electrode. The surface of the electrode underwent modification with molybdenum disulfide nanosheets (MoS₂NSs). Further, the interface was designed with molecularly imprinted polymer (MIP) targeting CRP. An electrochemical technique carefully examined the electrode at each modification stage. The created sensing interface can detect a wide concentration range from 0.01 nM to 100 nM, with a lower detection limit of 0.01 nM.

新生儿败血症是新生儿诱发的一种复杂的全身性疾病。多种真菌、病毒和细菌都会引发这种疾病。传统的方法，如放射成像、微生物检测、血液培养和炎症标志物等，在及时检测感染方面受到一系列限制。本研究展示了一种先进的智能电化学生物传感系统。该系统经过精心设计，可识别 C 反应蛋白 (CRP) 的浓度。CRP 是新生儿败血症不可替代的预后指标。这项工作阐述了在丝网印刷微型电极上制作生物受体传感平台（BioRe Sense）的过程。电极表面经过二硫化钼纳米片（MoS2NSs）修饰。此外，还设计了针对 CRP 的分子印迹聚合物（MIP）界面。电化学技术仔细检查了每个修饰阶段的电极。所创建的传感界面可检测 0.01 nM 至 100 nM 的宽浓度范围，检测下限为 0.01 nM。

{"title":"Advancing electrochemical sensing: A smart platform for accurate CRP level detection in neonatal septicaemia","authors":"Sapna Balayan , Nidhi Chauhan , Vinita Hooda , Ramesh Chandra , Warren Rosario , Utkarsh Jain","doi":"10.1016/j.talo.2024.100369","DOIUrl":"10.1016/j.talo.2024.100369","url":null,"abstract":"<div><div>Neonatal septicaemia is an intricate systemic affliction induced in newborns. A multitude of fungi, viruses, and bacteria elicit this condition. Conventional methodologies such as radiological imaging, microbial testing, blood culture, and inflammatory markers suffer from an array of constraints for prompt detection of infection. This present study illustrates a cutting-edge smart electrochemical biosensing system. The fabricated system was meticulously engineered to discern the concentration of C-reactive protein (CRP). CRP is an irreplaceable prognostic indicator for neonatal sepsis. This work explicates the fabrication of a bioreceptor sensing platform (BioRe Sense) on a screen-printed miniaturized electrode. The surface of the electrode underwent modification with molybdenum disulfide nanosheets (MoS<sub>2</sub>NSs). Further, the interface was designed with molecularly imprinted polymer (MIP) targeting CRP. An electrochemical technique carefully examined the electrode at each modification stage. The created sensing interface can detect a wide concentration range from 0.01 nM to 100 nM, with a lower detection limit of 0.01 nM.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100369"},"PeriodicalIF":4.1,"publicationDate":"2024-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142560755","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Progressive analytical techniques utilized for the detection of contaminants attributed to food safety and security 用于检测食品安全污染物的先进分析技术

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-18 DOI: 10.1016/j.talo.2024.100368

Anjali Bharti, Utkarsh Jain, Nidhi Chauhan

Food analysis and authentication are very crucial to assure safety, quality, and integrity of food and food-related products. Analysis of food products not only ensures the quality of food but also gives information about composition, physical characteristics, flavor, shelf-life, safety, microstructure, and processibility. Consequently, food is now regarded as an inexpensive means of preventing disease while also serving as a source of energy. Typically, a wide range of distinct chemical components make up the chemical composition of food. Furthermore, during processing or storage, food is always susceptible to structural alterations. Therefore, to assess the nutritional value and the quality of food products, food components must be analyzed and quantified. Food analysis mainly includes the preparation, examination, and identification of major food components, such as dietary fiber, phenolic compounds, carbohydrates, proteins, amino acids, peptides, enzymes, phospholipids, pesticides, alcohols, fat-soluble and water-soluble vitamins, organic acids, organic bases, bittering agents, pigments, and aroma compounds, as well as minor components including preservatives, antioxidants, colorants. Therefore, there are several advanced analytical techniques, including spectroscopy, mass spectrometry, chromatography, NMR, HSI, MALDI-TOF, RT-PCR, biosensors, etc. have been vital in the food science domain due to their high selectivity and sensitivity. This review emphasizes implementing various analytical techniques to analyze food safety and security.

食品分析和鉴定对于确保食品和食品相关产品的安全、质量和完整性至关重要。食品分析不仅能确保食品质量，还能提供有关成分、物理特性、风味、保质期、安全性、微观结构和加工性等方面的信息。因此，食品现在被视为一种预防疾病的廉价手段，同时也是一种能量来源。食品的化学成分通常由多种不同的化学成分组成。此外，在加工或储存过程中，食品的结构总是容易发生变化。因此，为了评估食品的营养价值和质量，必须对食品成分进行分析和量化。食品分析主要包括膳食纤维、酚类化合物、碳水化合物、蛋白质、氨基酸、肽、酶、磷脂、杀虫剂、醇类、脂溶性和水溶性维生素、有机酸、有机碱、苦味剂、色素和芳香化合物等主要食品成分，以及防腐剂、抗氧化剂、着色剂等次要成分的制备、检验和鉴定。因此，一些先进的分析技术，包括光谱、质谱、色谱、核磁共振、HSI、MALDI-TOF、RT-PCR、生物传感器等，因其高选择性和高灵敏度而在食品科学领域发挥着重要作用。本综述强调采用各种分析技术来分析食品安全和保障。

{"title":"Progressive analytical techniques utilized for the detection of contaminants attributed to food safety and security","authors":"Anjali Bharti, Utkarsh Jain, Nidhi Chauhan","doi":"10.1016/j.talo.2024.100368","DOIUrl":"10.1016/j.talo.2024.100368","url":null,"abstract":"<div><div>Food analysis and authentication are very crucial to assure safety, quality, and integrity of food and food-related products. Analysis of food products not only ensures the quality of food but also gives information about composition, physical characteristics, flavor, shelf-life, safety, microstructure, and processibility. Consequently, food is now regarded as an inexpensive means of preventing disease while also serving as a source of energy. Typically, a wide range of distinct chemical components make up the chemical composition of food. Furthermore, during processing or storage, food is always susceptible to structural alterations. Therefore, to assess the nutritional value and the quality of food products, food components must be analyzed and quantified. Food analysis mainly includes the preparation, examination, and identification of major food components, such as dietary fiber, phenolic compounds, carbohydrates, proteins, amino acids, peptides, enzymes, phospholipids, pesticides, alcohols, fat-soluble and water-soluble vitamins, organic acids, organic bases, bittering agents, pigments, and aroma compounds, as well as minor components including preservatives, antioxidants, colorants. Therefore, there are several advanced analytical techniques, including spectroscopy, mass spectrometry, chromatography, NMR, HSI, MALDI-TOF, RT-PCR, biosensors, etc. have been vital in the food science domain due to their high selectivity and sensitivity. This review emphasizes implementing various analytical techniques to analyze food safety and security.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100368"},"PeriodicalIF":4.1,"publicationDate":"2024-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592727","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Identification of potential volatile markers for characterizing Argentine wine vinegars based on their production process 根据生产工艺确定潜在的挥发性标记，以描述阿根廷葡萄酒醋的特征

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-18 DOI: 10.1016/j.talo.2024.100370

Marcelo Wagner , Jorgelina Zaldarriaga Heredia , M. Pilar Segura-Borrego , M. Lourdes Morales , José M. Camiña , Silvana M. Azcarate , Raquel M. Callejón , Rocío Ríos-Reina

In Argentina, the production of quality wine vinegars has been barely exploited. Currently, most of the marketed vinegars are produced using rapid industrial fermentation systems obtaining vinegars with a high production rate, but with low quality and few organoleptic nuances. This work aims to study the volatile profile by headspace solid phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC–MS) and chemometrics to differentiate Argentinian wine vinegars according to their production process (industrial or traditional). A total of 92 volatile compounds were identified on the samples by using a strategy based on volatile profile processing using PARADISe® software. The complete volatile profile of all the samples was submitted to partial least squares discriminant analysis (PLS-DA) for the selection of variables with importance in the projection (VIPs). Thus, 37 volatile compounds with the potential to be markers of the manufacturing process were selected. The results obtained revealed, for the first time, the volatile profile of Argentine wine vinegars showing that the compound groups that, on average, exhibited higher relative areas were esters, acids, and alcohols. Thus, certain acids, aldehydes and terpenes were noticeably present in industrial wine vinegar. Conversely, the alcohols were strongly associated with traditional ones. In the case of esters, they were connected to the different types of wine vinegars. These compounds could be considered as potential volatile markers of quality and authenticity of these types of vinegars.

在阿根廷，优质葡萄酒醋的生产几乎没有得到开发。目前，市场上销售的大多数葡萄酒醋都是通过快速工业发酵系统生产出来的，虽然产量高，但质量低，感官上的细微差别也很少。这项研究旨在通过顶空固相微萃取（HS-SPME）结合气相色谱-质谱联用仪（GC-MS）和化学计量学来研究挥发性成分，从而根据生产工艺（工业或传统）来区分阿根廷葡萄酒醋。通过 PARADISe® 软件的挥发性特征处理策略，对样品中的 92 种挥发性化合物进行了鉴定。所有样品的完整挥发性曲线都经过了偏最小二乘判别分析（PLS-DA），以筛选出在预测中具有重要意义的变量（VIPs）。因此，选出了 37 种有可能成为生产过程标记的挥发性化合物。研究结果首次揭示了阿根廷葡萄酒醋的挥发性特征，显示酯类、酸类和醇类化合物的平均相对含量较高。因此，工业葡萄酒醋中明显含有某些酸、醛和萜烯。相反，醇类则与传统酿造工艺密切相关。酯类则与不同类型的葡萄酒醋有关。这些化合物可被视为这些类型酒醋质量和真实性的潜在挥发性标记。

{"title":"Identification of potential volatile markers for characterizing Argentine wine vinegars based on their production process","authors":"Marcelo Wagner , Jorgelina Zaldarriaga Heredia , M. Pilar Segura-Borrego , M. Lourdes Morales , José M. Camiña , Silvana M. Azcarate , Raquel M. Callejón , Rocío Ríos-Reina","doi":"10.1016/j.talo.2024.100370","DOIUrl":"10.1016/j.talo.2024.100370","url":null,"abstract":"<div><div>In Argentina, the production of quality wine vinegars has been barely exploited. Currently, most of the marketed vinegars are produced using rapid industrial fermentation systems obtaining vinegars with a high production rate, but with low quality and few organoleptic nuances. This work aims to study the volatile profile by headspace solid phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC–MS) and chemometrics to differentiate Argentinian wine vinegars according to their production process (industrial or traditional). A total of 92 volatile compounds were identified on the samples by using a strategy based on volatile profile processing using PARADISe® software. The complete volatile profile of all the samples was submitted to partial least squares discriminant analysis (PLS-DA) for the selection of variables with importance in the projection (VIPs). Thus, 37 volatile compounds with the potential to be markers of the manufacturing process were selected. The results obtained revealed, for the first time, the volatile profile of Argentine wine vinegars showing that the compound groups that, on average, exhibited higher relative areas were esters, acids, and alcohols. Thus, certain acids, aldehydes and terpenes were noticeably present in industrial wine vinegar. Conversely, the alcohols were strongly associated with traditional ones. In the case of esters, they were connected to the different types of wine vinegars. These compounds could be considered as potential volatile markers of quality and authenticity of these types of vinegars.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100370"},"PeriodicalIF":4.1,"publicationDate":"2024-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533039","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Evaluating the greenness, blueness, and whiteness of spectroscopic and UPLC techniques for the simultaneous measurement of anti-glaucoma drugs and the preservation agent 评估光谱技术和超高效液相色谱技术同时测定抗青光眼药物和保存剂的绿色、蓝色和白色

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-18 DOI: 10.1016/j.talo.2024.100367

Eman A. Assirey , Noha S. katamesh , Mahmoud A. Mohamed

The pursuit of sustainable solutions is increasingly crucial in contemporary times. We propose inventive research that fulfills the criteria of whiteness and greenness in analytical chemistry. The endeavor aims to advance environmentally conscious techniques for the simultaneous detection of timolol maleate (TIM), dorzolamide HCl (DOR), and benzalkonium Cl (BNZ). The first method employed a sustainable mobile phase consisting of 0.02 M phosphate buffer: ethanol (68:32, v/v), and a flow rate of 0.6 mL/min with retention times 1.274, 1.798, and 2.483 min for DOR, TIM, and BNZ, respectively, with a UV detector at 210 nm. This methodology was easy, fast, and accurate. The approach showed low processing times, peak symmetry, and satisfactory resolution, with correlation values of 0.999. The linearity was between 0.001–0.064, 0.001–0.060 µg mL^-1, and 0.001–0.050 µg mL^-1for DOR, TIM, and BNZ, respectively. Furthermore, employing water as the solvent, complementary spectrophotometric methods such as Mean Centering of Ratio Spectra (MCR) and Successive Derivative Ratio Spectra (SRDS) were investigated as economical and environmentally friendly substitutes. All procedures demonstrated good linearity (r² > 0.9990), acceptable accuracy, and precision (RSD ≤ 2 %). Furthermore, by proving the superiority of the current work over previously published methods regarding sustainability, analytical performance, economics, and practicality, the real-world implementation of four greenness and whiteness algorithms boosts the approval and overall sustainable development of the proposed methods. The suggested techniques offer low-cost, environmentally friendly substitutes for traditional methods, advancing the field of analytical chemistry towards more sustainable practices and fostering a less destructive future for quality control.

在当代，追求可持续发展的解决方案越来越重要。我们建议开展创造性研究，以满足分析化学中的白色和绿色标准。这项工作旨在推进具有环保意识的同时检测马来酸噻吗洛尔（TIM）、盐酸多佐胺（DOR）和苯扎氯铵（BNZ）的技术。第一种方法采用的流动相为 0.02 M 磷酸盐缓冲液：乙醇（68:32, v/v），流速为 0.6 mL/min，DOR、TIM 和 BNZ 的保留时间分别为 1.274、1.798 和 2.483 min，紫外检测器的波长为 210 nm。该方法简便、快速、准确。该方法处理时间短，峰值对称，分辨率令人满意，相关值达到 0.999。DOR、TIM 和 BNZ 的线性范围分别为 0.001-0.064、0.001-0.060 µg mL-1 和 0.001-0.050 µg mL-1。此外，还研究了以水为溶剂的互补分光光度法，如平均中心比色光谱法（MCR）和连续衍生比色光谱法（SRDS），以作为经济、环保的替代方法。所有程序都表现出良好的线性（r² > 0.9990）、可接受的准确度和精确度（RSD ≤ 2 %）。此外，通过证明当前工作在可持续性、分析性能、经济性和实用性方面优于之前已发表的方法，四种绿色度和白度算法在现实世界中的实施促进了建议方法的认可和整体可持续发展。所建议的技术为传统方法提供了低成本、环保的替代品，推动分析化学领域朝着更可持续的方向发展，为质量控制创造一个破坏性更小的未来。

{"title":"Evaluating the greenness, blueness, and whiteness of spectroscopic and UPLC techniques for the simultaneous measurement of anti-glaucoma drugs and the preservation agent","authors":"Eman A. Assirey , Noha S. katamesh , Mahmoud A. Mohamed","doi":"10.1016/j.talo.2024.100367","DOIUrl":"10.1016/j.talo.2024.100367","url":null,"abstract":"<div><div>The pursuit of sustainable solutions is increasingly crucial in contemporary times. We propose inventive research that fulfills the criteria of whiteness and greenness in analytical chemistry. The endeavor aims to advance environmentally conscious techniques for the simultaneous detection of timolol maleate (TIM), dorzolamide HCl (DOR), and benzalkonium Cl (BNZ). The first method employed a sustainable mobile phase consisting of 0.02 M phosphate buffer: ethanol (68:32, v/v), and a flow rate of 0.6 mL/min with retention times 1.274, 1.798, and 2.483 min for DOR, TIM, and BNZ, respectively, with a UV detector at 210 nm. This methodology was easy, fast, and accurate. The approach showed low processing times, peak symmetry, and satisfactory resolution, with correlation values of 0.999. The linearity was between 0.001–0.064, 0.001–0.060 µg mL<sup>-1</sup>, and 0.001–0.050 µg mL<sup>-1</sup>for DOR, TIM, and BNZ, respectively. Furthermore, employing water as the solvent, complementary spectrophotometric methods such as Mean Centering of Ratio Spectra (MCR) and Successive Derivative Ratio Spectra (SRDS) were investigated as economical and environmentally friendly substitutes. All procedures demonstrated good linearity (r² > 0.9990), acceptable accuracy, and precision (RSD ≤ 2 %). Furthermore, by proving the superiority of the current work over previously published methods regarding sustainability, analytical performance, economics, and practicality, the real-world implementation of four greenness and whiteness algorithms boosts the approval and overall sustainable development of the proposed methods. The suggested techniques offer low-cost, environmentally friendly substitutes for traditional methods, advancing the field of analytical chemistry towards more sustainable practices and fostering a less destructive future for quality control.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100367"},"PeriodicalIF":4.1,"publicationDate":"2024-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533040","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Absolute mass spectrometry: A theoretical analytical technique for quantification 绝对质谱法：用于定量的理论分析技术

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-16 DOI: 10.1016/j.talo.2024.100366

Ignacio J. Rios, Fabiana C. Gennari

Mass spectrometry (MS) is an analytical chemistry technique that requires calibration with standards in order to quantify an analyte in a sample. In many cases the reference standards may be difficult to obtain or unavailable. In fact, when MS is applied to study reactions that yield multiple products, their quantification requires several standards and involves time-consuming and tedious calibration procedures. In other applications like Mass Spectrometry Imaging (MSI), quantification becomes even more tedious when on-tissue standards or mimetic tissue models are required. In this work, we introduce a new measurement technique that we called the Absolute Mass Spectrometry (AbMS), which allows the absolute quantification of an analyte without the need for calibration standards. This technique is based on the “Influence Method” developed in 2015 for nuclear measurements which, when applied to MS, produces this improvement for analyte quantification. Two possible applications of this technique are presented. One is the conceptual development of a mass spectrometer with electronic ionization that does not require calibration to determine the amount of analyte. The other one describes how to apply this technique in a mass spectrometer with other ionization sources like MALDI, DESI, and SIMS, which are used in MSI. AbMS technique uses the conceptual basis of Influence Method and two consecutive measurements to estimate the amount of analyte. Specifically, AbMS can be directly employed as an absolute method for quantification in MSI. Therefore, it constitutes an attractive complement for research applications in pharmaceutical and health sciences.

质谱法（MS）是一种分析化学技术，需要用标准物质进行校准，才能对样品中的分析物进行定量。在许多情况下，参考标准可能难以获得或无法获得。事实上，当质谱应用于研究产生多种产物的反应时，其定量需要多个标准，并涉及耗时而繁琐的校准程序。在质谱成像（MSI）等其他应用中，如果需要组织上的标准或模拟组织模型，定量工作就会变得更加繁琐。在这项工作中，我们引入了一种新的测量技术，称为绝对质谱法（AbMS），无需校准标准即可对分析物进行绝对定量。该技术基于 2015 年开发的用于核测量的 "影响法"，将其应用于质谱时，可改进分析物的定量。本文介绍了该技术的两种可能应用。其一是概念性地开发一种无需校准即可确定分析物含量的电子电离质谱仪。另一种是介绍如何在质谱仪中应用该技术，以及在 MSI 中使用的其他电离源，如 MALDI、DESI 和 SIMS。AbMS 技术利用影响法的概念基础和两次连续测量来估算分析物的含量。具体来说，AbMS 可直接用作 MSI 中的绝对定量方法。因此，它是制药和健康科学研究应用中一种极具吸引力的补充方法。

{"title":"Absolute mass spectrometry: A theoretical analytical technique for quantification","authors":"Ignacio J. Rios, Fabiana C. Gennari","doi":"10.1016/j.talo.2024.100366","DOIUrl":"10.1016/j.talo.2024.100366","url":null,"abstract":"<div><div>Mass spectrometry (MS) is an analytical chemistry technique that requires calibration with standards in order to quantify an analyte in a sample. In many cases the reference standards may be difficult to obtain or unavailable. In fact, when MS is applied to study reactions that yield multiple products, their quantification requires several standards and involves time-consuming and tedious calibration procedures. In other applications like Mass Spectrometry Imaging (MSI), quantification becomes even more tedious when on-tissue standards or mimetic tissue models are required. In this work, we introduce a new measurement technique that we called the Absolute Mass Spectrometry (AbMS), which allows the absolute quantification of an analyte without the need for calibration standards. This technique is based on the “Influence Method” developed in 2015 for nuclear measurements which, when applied to MS, produces this improvement for analyte quantification. Two possible applications of this technique are presented. One is the conceptual development of a mass spectrometer with electronic ionization that does not require calibration to determine the amount of analyte. The other one describes how to apply this technique in a mass spectrometer with other ionization sources like MALDI, DESI, and SIMS, which are used in MSI. AbMS technique uses the conceptual basis of Influence Method and two consecutive measurements to estimate the amount of analyte. Specifically, AbMS can be directly employed as an absolute method for quantification in MSI. Therefore, it constitutes an attractive complement for research applications in pharmaceutical and health sciences.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100366"},"PeriodicalIF":4.1,"publicationDate":"2024-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142533038","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A validated high-performance liquid chromatography-ultraviolet method for the determination of valproic acid derivatives in pharmaceutical formulations with a microbiological suitability evaluation 高效液相色谱-紫外法测定药物制剂中丙戊酸衍生物的有效方法及微生物适用性评估

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open

Pub Date : 2024-10-01 DOI: 10.1016/j.talo.2024.100365

Abdullah H. Alluhayb , Mostafa F. Al-Hakkani , Mahmoud Abdulnasser , Bandar R. Alsehli , Mohammed S. Saddik , Mohammad H.A. Hassan , Sayed M Saleh

Valproic acid and its derivatives are common drugs used in the treatment of epilepsy, a result of CNS disorders. Because the molecular structure of valproic acid, as a fatty acid, does not contain any chromophore groups, its peak response demanded special conditions to be detected in HPLC, ensuring the best precision results. Still, the current approach illustrates simple, validated procedures for conduction. The conducted chromatographic system consists of the BDS Hypersil C8, 150 × 4.6 mm, 5 µm column using a mobile phase of acetonitrile: phosphate buffer (4:6) at a detection wavelength of 215 nm at room temperature. A full method validation study was conducted and approved to ensure precise, repeatable, and accurate results by implementing system suitability parameters. In microbiological terms, a suitability test is used to validate microbiological testing methods, ensuring their efficacy despite potential interference from antimicrobial properties in the tested materials. The HPLC-UV developed and validated analytical method was evaluated, and it was found to be sensitive for use in the detection of low concentrations of methylparaben, propylparaben, and valproate with an optimum run time of six minutes. limit of detection (LODs) were statistically estimated and found to be 2.27 µg/mL, 39.77 ng/mL, and 1.84 µg/mL for methylparaben, propylparaben, and valproate, respectively. Additionally, the method demonstrated a high recovery of methylparaben, propylparaben, and valproate with an excellent closed-accuracy range (98.84% - 101.34%). An excellent regression coefficient (r) of 0.99924, 0.99998, and 0.99997 for methylparaben, valproate, and propylparaben, respectively, was achieved. Assay determination of various pharmaceutical dosage forms in the local market was implemented, yielding admirable results.

丙戊酸及其衍生物是治疗中枢神经系统疾病癫痫的常用药物。由于丙戊酸是一种脂肪酸，其分子结构中不含任何发色团，因此其峰值响应需要特殊条件才能在高效液相色谱法中检测到，以确保获得最佳精度结果。不过，目前的方法说明了简单、有效的传导程序。色谱系统采用 BDS Hypersil C8 色谱柱，150 × 4.6 mm，5 µm，流动相为乙腈：磷酸盐缓冲液（4:6），室温下检测波长为 215 nm。为确保检测结果的精确性、可重复性和准确性，我们进行了全面的方法验证研究，并通过了系统适用性参数的设置。从微生物学角度讲，适宜性测试用于验证微生物测试方法，确保这些方法在受测材料的抗菌特性可能造成干扰的情况下仍然有效。对开发和验证的 HPLC-UV 分析方法进行了评估，发现该方法灵敏度高，可用于检测低浓度的尼泊金甲酯、尼泊金丙酯和丙戊酸酯，最佳运行时间为 6 分钟。经统计估算，发现尼泊金甲酯、尼泊金丙酯和丙戊酸酯的检测限（LOD）分别为 2.27 µg/mL、39.77 ng/mL 和 1.84 µg/mL。此外，该方法还显示出对羟基苯甲酸甲酯、对羟基苯甲酸丙酯和丙戊酸钠的高回收率和极佳的闭合准确度范围（98.84% - 101.34%）。苯甲酸甲酯、丙戊酯和丙戊酯的回归系数（r）分别为 0.99924、0.99998 和 0.99997。对本地市场上的各种药物剂型进行了测定，结果令人满意。

{"title":"A validated high-performance liquid chromatography-ultraviolet method for the determination of valproic acid derivatives in pharmaceutical formulations with a microbiological suitability evaluation","authors":"Abdullah H. Alluhayb , Mostafa F. Al-Hakkani , Mahmoud Abdulnasser , Bandar R. Alsehli , Mohammed S. Saddik , Mohammad H.A. Hassan , Sayed M Saleh","doi":"10.1016/j.talo.2024.100365","DOIUrl":"10.1016/j.talo.2024.100365","url":null,"abstract":"<div><div>Valproic acid and its derivatives are common drugs used in the treatment of epilepsy, a result of CNS disorders. Because the molecular structure of valproic acid, as a fatty acid, does not contain any chromophore groups, its peak response demanded special conditions to be detected in HPLC, ensuring the best precision results. Still, the current approach illustrates simple, validated procedures for conduction. The conducted chromatographic system consists of the BDS Hypersil C8, 150 × 4.6 mm, 5 µm column using a mobile phase of acetonitrile: phosphate buffer (4:6) at a detection wavelength of 215 nm at room temperature. A full method validation study was conducted and approved to ensure precise, repeatable, and accurate results by implementing system suitability parameters. In microbiological terms, a suitability test is used to validate microbiological testing methods, ensuring their efficacy despite potential interference from antimicrobial properties in the tested materials. The HPLC-UV developed and validated analytical method was evaluated, and it was found to be sensitive for use in the detection of low concentrations of methylparaben, propylparaben, and valproate with an optimum run time of six minutes. limit of detection (LODs) were statistically estimated and found to be 2.27 µg/mL, 39.77 ng/mL, and 1.84 µg/mL for methylparaben, propylparaben, and valproate, respectively. Additionally, the method demonstrated a high recovery of methylparaben, propylparaben, and valproate with an excellent closed-accuracy range (98.84% - 101.34%). An excellent regression coefficient (r) of 0.99924, 0.99998, and 0.99997 for methylparaben, valproate, and propylparaben, respectively, was achieved. Assay determination of various pharmaceutical dosage forms in the local market was implemented, yielding admirable results.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100365"},"PeriodicalIF":4.1,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142426999","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0