Pub Date : 2024-02-02DOI: 10.3390/analytica5010005
A. E. F. Oliveira, Arnaldo César Pereira, Mayra A. C. Resende, L. F. Ferreira
A disposable voltammetric immunosensor was developed to measure breast cancer biomarker 15-3 (CA 15-3) in human saliva and serum samples. Screen-printed paper-based electrodes (f-SPE) previously fabricated by our research group using homemade conductive inks were used as transducers, which were later modified only with gold nanoparticles to immobilize anti-CA 15-3 antibodies. The sensor was operated using antigen–antibody interactions in conjunction with a redox species (ferrocyanide potassium) for the indirect determination of the CA 15-3 antigen. The device characterization involved atomic force microscopy (AFM) and electrochemical analysis. Optimization of the construction and response of the immunosensor was achieved at incubation times of 6 h for anti-CA 15-3, 1 h for bovine serum albumin, and 1 h for interaction with CA 15-3. The sensor displays a linear range between 2 and 16 U/mL, with a sensitivity of 0.012 μA/U mL−1, a limit of detection (LOD) of 0.56 U/mL, and a limit of quantification (LOQ) of 1.88 U/mL. The interfering substances minimally affected the signal, with 4.94% response variation, and the reproducibility of the immunosensor demonstrated a relative standard deviation (RSD) of 5.65%. The sensor successfully determined the CA 15-3 concentration in human serum and saliva, demonstrating its potential for clinical analysis.
我们开发了一种一次性伏安免疫传感器，用于测量人体唾液和血清样本中的乳腺癌生物标记物 15-3 (CA15-3)。我们的研究小组以前用自制导电油墨制作的丝网印刷纸基电极（f-SPE）被用作传感器，后来仅用金纳米粒子对其进行了修饰，以固定抗 CA 15-3 抗体。该传感器利用抗原-抗体之间的相互作用以及氧化还原物质（亚铁氰化钾）来间接测定 CA 15-3 抗原。该装置的表征包括原子力显微镜（AFM）和电化学分析。抗 CA 15-3 的孵育时间为 6 小时，牛血清白蛋白的孵育时间为 1 小时，与 CA 15-3 相互作用的孵育时间为 1 小时，在这些条件下对免疫传感器的构造和响应进行了优化。该传感器的线性范围为 2 至 16 U/mL，灵敏度为 0.012 μA/U mL-1，检出限（LOD）为 0.56 U/mL，定量限（LOQ）为 1.88 U/mL。干扰物质对信号的影响很小，反应变异率为 4.94%，免疫传感器的重现性相对标准偏差（RSD）为 5.65%。该传感器成功测定了人体血清和唾液中的 CA 15-3 浓度，证明了其在临床分析中的应用潜力。
{"title":"Disposable Voltammetric Immunosensor for Determination and Quantification of Biomarker CA 15-3 in Biological Specimens","authors":"A. E. F. Oliveira, Arnaldo César Pereira, Mayra A. C. Resende, L. F. Ferreira","doi":"10.3390/analytica5010005","DOIUrl":"https://doi.org/10.3390/analytica5010005","url":null,"abstract":"A disposable voltammetric immunosensor was developed to measure breast cancer biomarker 15-3 (CA 15-3) in human saliva and serum samples. Screen-printed paper-based electrodes (f-SPE) previously fabricated by our research group using homemade conductive inks were used as transducers, which were later modified only with gold nanoparticles to immobilize anti-CA 15-3 antibodies. The sensor was operated using antigen–antibody interactions in conjunction with a redox species (ferrocyanide potassium) for the indirect determination of the CA 15-3 antigen. The device characterization involved atomic force microscopy (AFM) and electrochemical analysis. Optimization of the construction and response of the immunosensor was achieved at incubation times of 6 h for anti-CA 15-3, 1 h for bovine serum albumin, and 1 h for interaction with CA 15-3. The sensor displays a linear range between 2 and 16 U/mL, with a sensitivity of 0.012 μA/U mL−1, a limit of detection (LOD) of 0.56 U/mL, and a limit of quantification (LOQ) of 1.88 U/mL. The interfering substances minimally affected the signal, with 4.94% response variation, and the reproducibility of the immunosensor demonstrated a relative standard deviation (RSD) of 5.65%. The sensor successfully determined the CA 15-3 concentration in human serum and saliva, demonstrating its potential for clinical analysis.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"84 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139869590","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-13DOI: 10.3390/analytica5010003
Suresh K. Nagumalli, Joshua T. Salley, Jeffrey D. Carstens
Echinacea, a herbaceous, perennial flowering plant from the Compositae (Asteraceae) family, exhibits stimulating effects on myeloid progenitors (CFU-GMs) in rat bone marrow, as demonstrated in our previous study using a 75% (v v−1) ethanol extract of aerial parts. Expanding on this work, we have investigated eleven different Echinacea samples that belong to three species for their myeloid progenitor-stimulating activity. Simultaneously, we employed 1H-NMR spectroscopy (400 MHz, 0.02–10.02 ppm) and chemometric analysis to predict constituents responsible for activity. Female Sprague–Dawley rats received oral doses of ethanol extracts (0–200 mg extract dry weight kg−1 body weight) of Echinacea for seven days. Bone marrow cells were then cultured with CFU-GM growth factors. Extracts showing a statistically significant (p < 0.05) increase in CFU-GM, compared to the control, were considered active. Significant CFU-GM increases were observed in rats treated with seven Echinacea samples, ranging from 39% to 91% higher than the control, while four samples were inactive. All five Echinacea purpurea samples showed myeloid progenitor-stimulating activity, while one sample each of Echinacea angustifolia and Echinacea pallida also exhibited the same activity. By applying orthogonal partial least squares discriminant analysis (OPLS-DA) to the 1H-NMR spectra, we identified specific spectral bins (0.70–1.98 ppm aliphatic and 6.38–7.76 ppm aromatic) correlating with myelopoiesis stimulation. These findings highlight the potential of chemometric analysis using 1H-NMR spectroscopy to infer the chemical classes that could be responsible for the bioactive properties of complex herbal mixtures, like Echinacea.
{"title":"1H-NMR-Based Chemometric Analysis of Echinacea Species to Predict Effectors of Myeloid Progenitor Stimulation","authors":"Suresh K. Nagumalli, Joshua T. Salley, Jeffrey D. Carstens","doi":"10.3390/analytica5010003","DOIUrl":"https://doi.org/10.3390/analytica5010003","url":null,"abstract":"Echinacea, a herbaceous, perennial flowering plant from the Compositae (Asteraceae) family, exhibits stimulating effects on myeloid progenitors (CFU-GMs) in rat bone marrow, as demonstrated in our previous study using a 75% (v v−1) ethanol extract of aerial parts. Expanding on this work, we have investigated eleven different Echinacea samples that belong to three species for their myeloid progenitor-stimulating activity. Simultaneously, we employed 1H-NMR spectroscopy (400 MHz, 0.02–10.02 ppm) and chemometric analysis to predict constituents responsible for activity. Female Sprague–Dawley rats received oral doses of ethanol extracts (0–200 mg extract dry weight kg−1 body weight) of Echinacea for seven days. Bone marrow cells were then cultured with CFU-GM growth factors. Extracts showing a statistically significant (p < 0.05) increase in CFU-GM, compared to the control, were considered active. Significant CFU-GM increases were observed in rats treated with seven Echinacea samples, ranging from 39% to 91% higher than the control, while four samples were inactive. All five Echinacea purpurea samples showed myeloid progenitor-stimulating activity, while one sample each of Echinacea angustifolia and Echinacea pallida also exhibited the same activity. By applying orthogonal partial least squares discriminant analysis (OPLS-DA) to the 1H-NMR spectra, we identified specific spectral bins (0.70–1.98 ppm aliphatic and 6.38–7.76 ppm aromatic) correlating with myelopoiesis stimulation. These findings highlight the potential of chemometric analysis using 1H-NMR spectroscopy to infer the chemical classes that could be responsible for the bioactive properties of complex herbal mixtures, like Echinacea.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"26 10","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139530984","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-09DOI: 10.3390/analytica5010002
Maria Tarapoulouzi, Natasha Logan, Mike Hardy, Holly Montgomery, S. Haughey, Christopher T Elliott, C. Theocharis
Halloumi cheese has recently gained a Protected Designation of Origin (PDO) indicator, which is related to the place (Cyprus) in which halloumi cheese is made. The PDO label is linked with several requirements, e.g., milk species, quantities, etc.; thus, it is important to study this product regarding authenticity. The utility of using two spectroscopic techniques, hyperspectral imaging (HSI) (400–1000 nm) and conventional near-infrared spectroscopy (NIR) (800–2500 nm) were assessed for the discrimination of 17 Cypriot halloumi cheese types, which could be categorized as of cow or goat–sheep origin. The aim of this study was to obtain spectral information for halloumi cheese using other promising infrared and imaging spectroscopic techniques as a comparison to a previously acquired mid-infrared (MIR) spectroscopy dataset. NIR and HSI are both fast and easy techniques in application, both of which provide significant information in food analysis. Chemometric analysis was crucial for interpreting the spectroscopic data by applying the unsupervised methods: principal component analysis (PCA) and hierarchical cluster analysis (HCA). The HSI model was found to be based intuitively on the appearance of cheese samples after freeze-drying (e.g., color; yellow/white, and texture; oily/dry), while the NIR grouping of samples was determined to be based on composition, mainly fat, protein and lactose content of the cheese samples. The HSI model returned distinct clusters of the two halloumi cheese types, cow and goat–sheep origin, with one outlier (16/17 accuracy; 94%), while the NIR model proved less accurate (13/17; 76%).
{"title":"A Pre-Trial Study to Identify Species of Origin in Halloumi Cheese Utilising Chemometrics with Near-Infrared and Hyperspectral Imaging Technologies","authors":"Maria Tarapoulouzi, Natasha Logan, Mike Hardy, Holly Montgomery, S. Haughey, Christopher T Elliott, C. Theocharis","doi":"10.3390/analytica5010002","DOIUrl":"https://doi.org/10.3390/analytica5010002","url":null,"abstract":"Halloumi cheese has recently gained a Protected Designation of Origin (PDO) indicator, which is related to the place (Cyprus) in which halloumi cheese is made. The PDO label is linked with several requirements, e.g., milk species, quantities, etc.; thus, it is important to study this product regarding authenticity. The utility of using two spectroscopic techniques, hyperspectral imaging (HSI) (400–1000 nm) and conventional near-infrared spectroscopy (NIR) (800–2500 nm) were assessed for the discrimination of 17 Cypriot halloumi cheese types, which could be categorized as of cow or goat–sheep origin. The aim of this study was to obtain spectral information for halloumi cheese using other promising infrared and imaging spectroscopic techniques as a comparison to a previously acquired mid-infrared (MIR) spectroscopy dataset. NIR and HSI are both fast and easy techniques in application, both of which provide significant information in food analysis. Chemometric analysis was crucial for interpreting the spectroscopic data by applying the unsupervised methods: principal component analysis (PCA) and hierarchical cluster analysis (HCA). The HSI model was found to be based intuitively on the appearance of cheese samples after freeze-drying (e.g., color; yellow/white, and texture; oily/dry), while the NIR grouping of samples was determined to be based on composition, mainly fat, protein and lactose content of the cheese samples. The HSI model returned distinct clusters of the two halloumi cheese types, cow and goat–sheep origin, with one outlier (16/17 accuracy; 94%), while the NIR model proved less accurate (13/17; 76%).","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"94 6","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139444527","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-02DOI: 10.3390/analytica5010001
Alina Pyka-Pająk
A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in the same sample. Among all the tested chromatographic conditions, the mixture consisting of chloroform + toluene + ethyl acetate + ethanol + acetic acid (18:18:7.5:5.0:0.3, v/v/v/v/v) and a silica gel 60F254 plate proved to be the most effective for the separation of the three tested active pharmaceutical ingredients (APIs) and substances related to paracetamol. The full validation of the proposed NP-TLC method proved that it is specific, precise, accurate, robust and sensitive. The percentage content in relation to the content declared by the manufacturer was for propyphenazone 99.8%, paracetamol 101.6% and caffeine 100.8%, which was in accordance with pharmacopoeial requirements. The results presented indicate the possibility of using the developed method in the routine control of pharmaceutical preparations containing these APIs. The proposed method is economical and more sensitive compared to the previously proposed planar methods for the simultaneous determination of APIs. What is more, the presented method may be an excellent economical alternative when the HPLC method is unavailable for such a determination.
{"title":"Determination of the Active Pharmaceutical Ingredients in Saridon Tablets Using an Economical and Sensitive Thin Layer Chromatography Method Combined with Densitometry","authors":"Alina Pyka-Pająk","doi":"10.3390/analytica5010001","DOIUrl":"https://doi.org/10.3390/analytica5010001","url":null,"abstract":"A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in the same sample. Among all the tested chromatographic conditions, the mixture consisting of chloroform + toluene + ethyl acetate + ethanol + acetic acid (18:18:7.5:5.0:0.3, v/v/v/v/v) and a silica gel 60F254 plate proved to be the most effective for the separation of the three tested active pharmaceutical ingredients (APIs) and substances related to paracetamol. The full validation of the proposed NP-TLC method proved that it is specific, precise, accurate, robust and sensitive. The percentage content in relation to the content declared by the manufacturer was for propyphenazone 99.8%, paracetamol 101.6% and caffeine 100.8%, which was in accordance with pharmacopoeial requirements. The results presented indicate the possibility of using the developed method in the routine control of pharmaceutical preparations containing these APIs. The proposed method is economical and more sensitive compared to the previously proposed planar methods for the simultaneous determination of APIs. What is more, the presented method may be an excellent economical alternative when the HPLC method is unavailable for such a determination.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"141 25","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139453113","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-05DOI: 10.3390/analytica4040036
Diana Fimbres-Olivarría, J. Marquez-Escalante, K. Martínez-Robinson, Valeria Miranda-Arizmendi, Y. D. Anda-Flores, A. Rascón-Chu, F. Brown‐Bojorquez, E. Carvajal‐Millan
Marine algae are a valuable source of polysaccharides. However, the information available on sulfated polysaccharides from microalgae is limited. Navicula sp. is a microalga present in the Sea of Cortez, of which little is known regarding their polysaccharides’ properties. This study investigated the physicochemical and microstructural characteristics of Navicula sp. sulfated polysaccharide (NSP). The Fourier transform infrared spectrum of NSP showed distinctive bands (1225 and 820 cm−1, assigned to S–O and C–O–S stretching, respectively), confirming the molecular identity. NSP registered molecular weight, intrinsic viscosity, a radius of gyration, and a hydrodynamic radius of 1650 kDa, 197 mL/g, 61 nm, and 36 nm, respectively. The zeta potential, electrophoretic mobility, conductivity, and diffusion coefficient of the molecule were −5.8 mV, −0.45 µm cm/s V, 0.70 mS/cm, and 2.9 × 10−9 cm2/s, respectively. The characteristic ratio and persistence length calculated for NSP were 4.2 and 1.3 nm, suggesting a nonstiff polysaccharide chain conformation. The Mark–Houwink–Sakurada α and K constants were 0.5 and 1.67 × 10−1, respectively, indicating a molecular random coil structure. NSP scanning electron microscopy revealed a rough and porous surface. Knowing these polysaccharides’ physicochemical and microstructural characteristics can be the starting point for elucidating their structure–function relationship as a valuable tool in advanced biomaterial design.
{"title":"Physicochemical and Microstructural Characteristics of Sulfated Polysaccharide from Marine Microalga","authors":"Diana Fimbres-Olivarría, J. Marquez-Escalante, K. Martínez-Robinson, Valeria Miranda-Arizmendi, Y. D. Anda-Flores, A. Rascón-Chu, F. Brown‐Bojorquez, E. Carvajal‐Millan","doi":"10.3390/analytica4040036","DOIUrl":"https://doi.org/10.3390/analytica4040036","url":null,"abstract":"Marine algae are a valuable source of polysaccharides. However, the information available on sulfated polysaccharides from microalgae is limited. Navicula sp. is a microalga present in the Sea of Cortez, of which little is known regarding their polysaccharides’ properties. This study investigated the physicochemical and microstructural characteristics of Navicula sp. sulfated polysaccharide (NSP). The Fourier transform infrared spectrum of NSP showed distinctive bands (1225 and 820 cm−1, assigned to S–O and C–O–S stretching, respectively), confirming the molecular identity. NSP registered molecular weight, intrinsic viscosity, a radius of gyration, and a hydrodynamic radius of 1650 kDa, 197 mL/g, 61 nm, and 36 nm, respectively. The zeta potential, electrophoretic mobility, conductivity, and diffusion coefficient of the molecule were −5.8 mV, −0.45 µm cm/s V, 0.70 mS/cm, and 2.9 × 10−9 cm2/s, respectively. The characteristic ratio and persistence length calculated for NSP were 4.2 and 1.3 nm, suggesting a nonstiff polysaccharide chain conformation. The Mark–Houwink–Sakurada α and K constants were 0.5 and 1.67 × 10−1, respectively, indicating a molecular random coil structure. NSP scanning electron microscopy revealed a rough and porous surface. Knowing these polysaccharides’ physicochemical and microstructural characteristics can be the starting point for elucidating their structure–function relationship as a valuable tool in advanced biomaterial design.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"10 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138600865","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-04DOI: 10.3390/analytica4040035
Thaís Cristina Cândido, Arnaldo César Pereira, Daniela Nunes da Silva
This work developed a conductive ink composed of carbonaceous material for printing electrochemical sensors. The optimized ink comprises graphite, carbon black, and nail polish, respectively (35.3:11.7:53%), as well as acetone as a solvent. The proportion was optimized with consideration of the binder’s solubilization, the ink’s suitability for the screen-printing process, and lower electrical resistance. The materials used, and the resulting ink, were analyzed by way of Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Raman spectroscopy, electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The charge transfer resistance (Rct) obtained was 0.348 kΩ. The conductive ink was used to print an electrode on a PET substrate, and a flexible and disposable electrode was obtained. The electroactive area obtained was 13.7 cm2, which was calculated by the Randles-Sevcik equation. The applicability of the device was demonstrated with a redox probe, providing a sensitivity of 0.02 µ A L mmol−1. The conductive ink has adequate homogeneity for producing electrodes using the screen-printing technique, with a low estimated production cost of $ 0.09 mL−1.
本工作研制了一种用于印刷电化学传感器的碳质材料导电油墨。优化后的油墨分别由石墨、炭黑和指甲油组成(35.3:11.7:53%)，丙酮为溶剂。考虑粘合剂的增溶性、油墨对丝网印刷工艺的适应性和较低的电阻，优化了配比。采用傅里叶变换红外光谱(FT-IR)、扫描电镜(SEM)、拉曼光谱(Raman)、电化学阻抗谱(EIS)和循环伏安法(CV)对所用材料和墨水进行了分析。所得电荷转移电阻(Rct)为0.348 kΩ。利用导电油墨在PET基板上打印电极，得到了柔性的一次性电极。得到的电活性面积为13.7 cm2，由Randles-Sevcik方程计算。通过氧化还原探针验证了该装置的适用性，灵敏度为0.02µa L mmol−1。导电油墨具有足够的均匀性，可以使用丝网印刷技术生产电极，估计生产成本为0.09 mL - 1美元。
{"title":"Development and Characterization of Conductive Ink Composed of Graphite and Carbon Black for Application in Printed Electrodes","authors":"Thaís Cristina Cândido, Arnaldo César Pereira, Daniela Nunes da Silva","doi":"10.3390/analytica4040035","DOIUrl":"https://doi.org/10.3390/analytica4040035","url":null,"abstract":"This work developed a conductive ink composed of carbonaceous material for printing electrochemical sensors. The optimized ink comprises graphite, carbon black, and nail polish, respectively (35.3:11.7:53%), as well as acetone as a solvent. The proportion was optimized with consideration of the binder’s solubilization, the ink’s suitability for the screen-printing process, and lower electrical resistance. The materials used, and the resulting ink, were analyzed by way of Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Raman spectroscopy, electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The charge transfer resistance (Rct) obtained was 0.348 kΩ. The conductive ink was used to print an electrode on a PET substrate, and a flexible and disposable electrode was obtained. The electroactive area obtained was 13.7 cm2, which was calculated by the Randles-Sevcik equation. The applicability of the device was demonstrated with a redox probe, providing a sensitivity of 0.02 µ A L mmol−1. The conductive ink has adequate homogeneity for producing electrodes using the screen-printing technique, with a low estimated production cost of $ 0.09 mL−1.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"57 20","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138604814","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-12-02DOI: 10.3390/analytica4040034
R. Aissa, Abderrahim Asbbane, Samira Oubannin, Laila Bijla, Zahra Bousaid, Otmane Hallouch, S. El Harkaoui, Bertrand Matthaeus, E. Sakar, S. Gharby
Argan kernels, fruits regurgitated by goats, are 30% cheaper than the regular kernels used to prepare food argan oil. The use of such argan kernels as a cosmetic ingredient, after refining, is thus economically attractive. The oxidative stability of argan oil prepared from sub-quality kernels is not known. In the present paper, the physicochemical quality, oxidative stability indices, and bioactive compounds of refined argan oil (RAO) obtained from sub-quality kernels and virgin argan oil (VAO) were compared and evaluated over a period of storage of 12 weeks at 60 °C. Quality parameters consisted of free fatty acids (FFAs), peroxide value (PV), p-anisidine value (p-AV), UV extinction coefficients (K232 and K270), total oxidation, iodine and saponification values, induction time, fatty acid composition, and tocopherol content. Our outcomes reveal that the combined effects of refining and storage generally resulted in high values of the routinely measured quality indices, including FFA, p-AV, K270, K232, and PV. Likewise, refining reduced the levels of individual tocopherols and unsaturated fatty acids (USFAs) but increased saturated fatty acids (SFAs). Similar trends were observed under storage with decreased levels of tocopherols and high SFA for both RAO and VAO. Storage also resulted in an increased level of USFAs in the case of RAO but not in VAO. The obtained results show that RAO was more sensitive to oxidation than VAO. At room temperature, RAO had a shorter induction time of six months, implying that RAO will have a shorter shelf life compared to VAR. Thus, such instability means that the refining process for argan oil must be carried out with great care, and this oil needs to be protected once refined.
{"title":"Oxidative Stability of Virgin and Refined Argan [Argania spinosa L. (Skeels)] Oil under Accelerated Aging Conditions and Shelf-Life Prediction at Room Temperature: A Comparative Study","authors":"R. Aissa, Abderrahim Asbbane, Samira Oubannin, Laila Bijla, Zahra Bousaid, Otmane Hallouch, S. El Harkaoui, Bertrand Matthaeus, E. Sakar, S. Gharby","doi":"10.3390/analytica4040034","DOIUrl":"https://doi.org/10.3390/analytica4040034","url":null,"abstract":"Argan kernels, fruits regurgitated by goats, are 30% cheaper than the regular kernels used to prepare food argan oil. The use of such argan kernels as a cosmetic ingredient, after refining, is thus economically attractive. The oxidative stability of argan oil prepared from sub-quality kernels is not known. In the present paper, the physicochemical quality, oxidative stability indices, and bioactive compounds of refined argan oil (RAO) obtained from sub-quality kernels and virgin argan oil (VAO) were compared and evaluated over a period of storage of 12 weeks at 60 °C. Quality parameters consisted of free fatty acids (FFAs), peroxide value (PV), p-anisidine value (p-AV), UV extinction coefficients (K232 and K270), total oxidation, iodine and saponification values, induction time, fatty acid composition, and tocopherol content. Our outcomes reveal that the combined effects of refining and storage generally resulted in high values of the routinely measured quality indices, including FFA, p-AV, K270, K232, and PV. Likewise, refining reduced the levels of individual tocopherols and unsaturated fatty acids (USFAs) but increased saturated fatty acids (SFAs). Similar trends were observed under storage with decreased levels of tocopherols and high SFA for both RAO and VAO. Storage also resulted in an increased level of USFAs in the case of RAO but not in VAO. The obtained results show that RAO was more sensitive to oxidation than VAO. At room temperature, RAO had a shorter induction time of six months, implying that RAO will have a shorter shelf life compared to VAR. Thus, such instability means that the refining process for argan oil must be carried out with great care, and this oil needs to be protected once refined.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"110 20","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138607952","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-11-07DOI: 10.3390/analytica4040033
Francielly T. Souto, Gleiston G. Dias
Optical detection devices have become an analytical tool of interest in diverse fields of science. The search for methods to identify and quantify different compounds has transposed this curiosity into a necessity, since some constituents threaten the safety of life in all its forms. In this context, 30 years ago, Prof. Prasanna de Silva presented the idea of sensors as Molecular Logic Gates (MLGs): a molecule that performs a logical operation based on one or more inputs (analytes) resulting in an output (optical modification such as fluorescence or absorption). In this review, we explore the implementation of MLGs based on the interference of a second input (second analyte) in suppressing or even blocking a first input (first analyte), often resulting in INHIBIT-type gates. This approach is interesting because it is not related to attached detecting groups in the MLG but to the relation between the first and the second input. In this sense, flexible and versatile MLGs can be straightforwardly designed based on input selection. To illustrate these cases, we selected examples seeking to diversify the inputs (first analytes and interfering analytes), outputs (turn on, turn off), optical response (fluorescent/colorimetric), and applicability of these MLGs.
光学探测装置已成为各个科学领域都感兴趣的分析工具。寻找识别和量化不同化合物的方法已经把这种好奇心变成了一种必需品，因为一些成分以各种形式威胁着生命的安全。在此背景下，30年前，Prasanna de Silva教授提出了传感器作为分子逻辑门(mlg)的想法:一种基于一个或多个输入(分析物)执行逻辑操作的分子，从而产生输出(荧光或吸收等光学修饰)。在这篇综述中，我们探讨了基于第二输入(第二分析物)的干扰来抑制甚至阻断第一输入(第一分析物)的mlg的实现，通常导致inhibition型门。这种方法很有趣，因为它与MLG中附加的检测组无关，而是与第一个和第二个输入之间的关系有关。从这个意义上说，灵活和通用的mlg可以根据输入选择直接设计。为了说明这些情况，我们选择了一些例子来寻求多样化的输入(第一分析物和干扰分析物)，输出(打开，关闭)，光学响应(荧光/比色)，以及这些mlg的适用性。
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Pub Date : 2023-11-06DOI: 10.3390/analytica4040031
Nawagamu A. K. Rajitha Perera, Sindhu K. Shankar, Cynthia M. Archambault, Vladimir N. Nesterov, Sreekar B. Marpu, Hao Yan, Mohammad A. Omary
A novel Eu(tta)3([4,4′-(t-bu)2-2,2′-bpy)] complex (tta-thenoyltrifluoroacetone), a ratiometric luminescent-based optical sensor for the quantitative determination of aluminum ion, is synthesized and characterized using XRD and 1H NMR. The XRD data reveal the slightly distorted octahedral structure. The complex displays a bright red emission at 613 nm in methanol which is characteristic of europium (III) complexes. Upon the addition of Al3+ ions, the red emission disappears, and a new blue emission at 398 nm emerges, manifesting the ratiometric nature of the complex. The turn-off of the red emission and turn-on of the blue emission are attributed to Eu-Al trans-metalation, as supported by Raman data that show the emergence of Al-O vibrations at 418, 495, and 608 cm−1 concomitant with the disappearance of Eu-O and Eu-N bond vibrations. Most aluminum sensors are known to suffer from interferences from other metals including Cu2+, Co2+, and Cd2+. However, the sensor reported here is tested for 11 common cations and shows no interference on sensitivity. To the best of our knowledge, this is the first known Eu-based luminescence sensor that successfully exhibited the ability to detect aluminum ions in ppb levels in aqueous environments. The calculated Al3+ binding constant is 2.496 × 103 ± 172. The complex shows a linear relationship in the range of 0–47.6 ppb (1.76 × 10−6 M) Al3+ and the limit of detection (LOD) is 4.79 ppb (1.77 × 10−7 M) in MeOH. ICP-OES is used for validation of the sensor complex in water and then it was used for quantitative detection of Al3+ ions in water as a real-life application. The complex can accurately detect Al3+ ions in the range of 4.97–24.9 ppb (1.84 × 10−7 M–9.2 × 10−7 M) with an LOD of 8.11 ppb (2.99 × 10−7 M). Considering that the aluminum ion serves no recognized function within the human body, its accumulation can lead to severe neurological disorders, including Parkinson’s and Alzheimer’s diseases. With the LOD value significantly lower than the WHO-recommended maximum permissible level of 200 ppb for aluminum in drinking water, even without high-power laser-aided signal enhancement, the sensor shows promise for detecting trace amounts of aluminum contamination in water. Therefore, it can significantly aid in the monitoring of even the smallest aluminum ion contamination in drinking water, industrial effluents, and natural water bodies.
{"title":"A Novel ppb-Level Sensitive and Highly Selective Europium-Based Diketone Luminescent Sensor for the Quantitative Detection of Aluminum Ions in Water Samples","authors":"Nawagamu A. K. Rajitha Perera, Sindhu K. Shankar, Cynthia M. Archambault, Vladimir N. Nesterov, Sreekar B. Marpu, Hao Yan, Mohammad A. Omary","doi":"10.3390/analytica4040031","DOIUrl":"https://doi.org/10.3390/analytica4040031","url":null,"abstract":"A novel Eu(tta)3([4,4′-(t-bu)2-2,2′-bpy)] complex (tta-thenoyltrifluoroacetone), a ratiometric luminescent-based optical sensor for the quantitative determination of aluminum ion, is synthesized and characterized using XRD and 1H NMR. The XRD data reveal the slightly distorted octahedral structure. The complex displays a bright red emission at 613 nm in methanol which is characteristic of europium (III) complexes. Upon the addition of Al3+ ions, the red emission disappears, and a new blue emission at 398 nm emerges, manifesting the ratiometric nature of the complex. The turn-off of the red emission and turn-on of the blue emission are attributed to Eu-Al trans-metalation, as supported by Raman data that show the emergence of Al-O vibrations at 418, 495, and 608 cm−1 concomitant with the disappearance of Eu-O and Eu-N bond vibrations. Most aluminum sensors are known to suffer from interferences from other metals including Cu2+, Co2+, and Cd2+. However, the sensor reported here is tested for 11 common cations and shows no interference on sensitivity. To the best of our knowledge, this is the first known Eu-based luminescence sensor that successfully exhibited the ability to detect aluminum ions in ppb levels in aqueous environments. The calculated Al3+ binding constant is 2.496 × 103 ± 172. The complex shows a linear relationship in the range of 0–47.6 ppb (1.76 × 10−6 M) Al3+ and the limit of detection (LOD) is 4.79 ppb (1.77 × 10−7 M) in MeOH. ICP-OES is used for validation of the sensor complex in water and then it was used for quantitative detection of Al3+ ions in water as a real-life application. The complex can accurately detect Al3+ ions in the range of 4.97–24.9 ppb (1.84 × 10−7 M–9.2 × 10−7 M) with an LOD of 8.11 ppb (2.99 × 10−7 M). Considering that the aluminum ion serves no recognized function within the human body, its accumulation can lead to severe neurological disorders, including Parkinson’s and Alzheimer’s diseases. With the LOD value significantly lower than the WHO-recommended maximum permissible level of 200 ppb for aluminum in drinking water, even without high-power laser-aided signal enhancement, the sensor shows promise for detecting trace amounts of aluminum contamination in water. Therefore, it can significantly aid in the monitoring of even the smallest aluminum ion contamination in drinking water, industrial effluents, and natural water bodies.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"11 9","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135589618","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-11-06DOI: 10.3390/analytica4040032
Grażyna Wejnerowska, Izabela Narloch
Chemical ultraviolet filters are widely used in a variety of cosmetic products to protect the skin from the harmful effects of UV radiation. In order to guarantee consumers’ health, the content in sunscreens is regulated in a number of countries. Many analytical methods are used to determine UV filters in cosmetics samples. In recent years, attention has been paid to the fact that the methods should have a small impact on the environment. This work examined the greenness of 10 reported chromatographic methods in the literature for the determination of UV filters in cosmetic samples using two new tools: analytical greenness metric (AGREE) and analytical greenness metric for sample preparation (AGREEprep). Microextraction methods of sample preparation in the AGREEprep assessment show a higher score of greenness. The results recommended the use of both tools to assess the greening of methods before planning laboratory analytical methods to measure their ecological impact on the environment.
{"title":"Comparison of the Greenness Assessment of Chromatographic Methods Used for Analysis of UV Filters in Cosmetic Samples","authors":"Grażyna Wejnerowska, Izabela Narloch","doi":"10.3390/analytica4040032","DOIUrl":"https://doi.org/10.3390/analytica4040032","url":null,"abstract":"Chemical ultraviolet filters are widely used in a variety of cosmetic products to protect the skin from the harmful effects of UV radiation. In order to guarantee consumers’ health, the content in sunscreens is regulated in a number of countries. Many analytical methods are used to determine UV filters in cosmetics samples. In recent years, attention has been paid to the fact that the methods should have a small impact on the environment. This work examined the greenness of 10 reported chromatographic methods in the literature for the determination of UV filters in cosmetic samples using two new tools: analytical greenness metric (AGREE) and analytical greenness metric for sample preparation (AGREEprep). Microextraction methods of sample preparation in the AGREEprep assessment show a higher score of greenness. The results recommended the use of both tools to assess the greening of methods before planning laboratory analytical methods to measure their ecological impact on the environment.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"63 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135635716","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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