Abstract Ibrutinib is a drug used for the treatment of marginal zone lymphoma, mantle cell lymphoma, lymphocytic leukemia, chronic graft, and Waldenstrom macroglobulinemia. A simple, sensitive, and fast liquid chromatographic and spectrophotometric method for the quantification of ibrutinib in pharmaceutical forms and bulk was developed and validated. The chromatographic technique was developed using an ODS 3 C 18 (250 mm × 4.6 mm i.d., 5 µm) column. The mobile phase was a mixture of 0.1% trifluoroacetic acid in water and acetonitrile (50/50, v/v) at a flow rate of 1.0 mL·min−1. Eluent detection was carried out at a wavelength of 260 nm using a ultraviolet detector. The retention time of ibrutinib was found to be 5.27. On the other hand, Ibrutinib was determined using a spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 260 nm. The developed techniques were validated in accordance with the protocols outlined in International conference on harmonisation of technical requirements for registration of pharmaceuticals for human (ICH) guidelines Q2(R1). Correlation coefficients for both methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1. The relative standard deviation values were low in intraday and interday precision tests. The accuracy of the developed techniques ranged 99.74–100.23% for the chromatographic method and 99.32–100.76% for the spectrophotometric method. The limits of detection and quantitation were 0.90 and 2.80 µg·mL−1 for the chromatographic method and 1.10 and 3.20 µg·mL−1 for the spectrophotometric method. The developed and validated analytical methods can be safely used in quality control tests for the determination of the amount of ibrutinib in pharmaceutical products.
伊鲁替尼是一种用于治疗边缘带淋巴瘤、套细胞淋巴瘤、淋巴细胞白血病、慢性移植物和Waldenstrom巨球蛋白血症的药物。建立了一种简便、灵敏、快速的液相色谱和分光光度法定量测定依鲁替尼制剂和散装制剂的方法。色谱技术采用ODS 3c 18 (250 mm × 4.6 mm, 5µm)色谱柱。流动相为0.1%三氟乙酸水溶液与乙腈(50/50,v/v)的混合物，流速为1.0 mL·min−1。用紫外检测器在波长260 nm处对洗脱液进行检测。依鲁替尼的保留时间为5.27。另一方面，通过测量溶液在260 nm波长处的吸光度，采用分光光度法测定伊鲁替尼。所开发的技术根据国际人用药品注册技术要求协调会议(ICH)指南Q2(R1)中概述的协议进行了验证。在5 ~ 30 mg·mL−1浓度范围内，两种方法的相关系数均大于0.999。日间和日间精密度试验的相对标准偏差值较低。色谱法的准确度为99.74 ~ 100.23%，分光光度法的准确度为99.32 ~ 100.76%。色谱法的检出限和定量限分别为0.90和2.80µg·mL−1，分光光度法的检出限和定量限分别为1.10和3.20µg·mL−1。开发和验证的分析方法可以安全地用于质量控制测试，以确定药品中伊鲁替尼的含量。
{"title":"Alternative analytical methods for ibrutinib quantification in pharmaceutical formulation: A statistical comparison","authors":"Erten Akbel, S. Güngör, I. Bulduk","doi":"10.1515/revac-2022-0039","DOIUrl":"https://doi.org/10.1515/revac-2022-0039","url":null,"abstract":"Abstract Ibrutinib is a drug used for the treatment of marginal zone lymphoma, mantle cell lymphoma, lymphocytic leukemia, chronic graft, and Waldenstrom macroglobulinemia. A simple, sensitive, and fast liquid chromatographic and spectrophotometric method for the quantification of ibrutinib in pharmaceutical forms and bulk was developed and validated. The chromatographic technique was developed using an ODS 3 C 18 (250 mm × 4.6 mm i.d., 5 µm) column. The mobile phase was a mixture of 0.1% trifluoroacetic acid in water and acetonitrile (50/50, v/v) at a flow rate of 1.0 mL·min−1. Eluent detection was carried out at a wavelength of 260 nm using a ultraviolet detector. The retention time of ibrutinib was found to be 5.27. On the other hand, Ibrutinib was determined using a spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 260 nm. The developed techniques were validated in accordance with the protocols outlined in International conference on harmonisation of technical requirements for registration of pharmaceuticals for human (ICH) guidelines Q2(R1). Correlation coefficients for both methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1. The relative standard deviation values were low in intraday and interday precision tests. The accuracy of the developed techniques ranged 99.74–100.23% for the chromatographic method and 99.32–100.76% for the spectrophotometric method. The limits of detection and quantitation were 0.90 and 2.80 µg·mL−1 for the chromatographic method and 1.10 and 3.20 µg·mL−1 for the spectrophotometric method. The developed and validated analytical methods can be safely used in quality control tests for the determination of the amount of ibrutinib in pharmaceutical products.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"15 1","pages":"146 - 157"},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78882555","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract An improved management of secondary raw materials (SRM) is a crucial contribution for a circular economy and necessitates knowledge about the composition of wastes and SRM. However, this information is scarce and has to be determined with chemical analysis (CA). CA of SRM faces challenges, which can be approached by using round robin tests (RRT) to identify deviations from the “true value” of an element/molecule content. An RRT is a testing approach, which involves multiple labs to analyze one or more samples and evaluates the lab results with regard to the goal of the RRT. This article presents a systematic literature review and investigates which purposes and which performance parameters (PP) are commonly applied in RRT of SRM. The examined literature shows that the two main purposes applied are assessment of method performance and assessment of lab performance. PP can be categorized into trueness performance parameters (TPP; assessing the deviation of a value from a reference value) and precision performance parameters (PPP; describing the variability of a data set). The main TPP identified are z score and relative deviation, the main PPP identified are standard deviation and relative standard deviation. These results offer the conclusions that RRT can be used as a bespoke method to deal with analytical effects and that the selection of PP for an RRT could be based on simplicity.
{"title":"Round robin tests of secondary raw materials: A systematic review of performance parameters","authors":"N. Korf, P. Mählitz, V. S. Rotter","doi":"10.1515/revac-2022-0033","DOIUrl":"https://doi.org/10.1515/revac-2022-0033","url":null,"abstract":"Abstract An improved management of secondary raw materials (SRM) is a crucial contribution for a circular economy and necessitates knowledge about the composition of wastes and SRM. However, this information is scarce and has to be determined with chemical analysis (CA). CA of SRM faces challenges, which can be approached by using round robin tests (RRT) to identify deviations from the “true value” of an element/molecule content. An RRT is a testing approach, which involves multiple labs to analyze one or more samples and evaluates the lab results with regard to the goal of the RRT. This article presents a systematic literature review and investigates which purposes and which performance parameters (PP) are commonly applied in RRT of SRM. The examined literature shows that the two main purposes applied are assessment of method performance and assessment of lab performance. PP can be categorized into trueness performance parameters (TPP; assessing the deviation of a value from a reference value) and precision performance parameters (PPP; describing the variability of a data set). The main TPP identified are z score and relative deviation, the main PPP identified are standard deviation and relative standard deviation. These results offer the conclusions that RRT can be used as a bespoke method to deal with analytical effects and that the selection of PP for an RRT could be based on simplicity.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"26 1","pages":"98 - 111"},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91322699","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract This study was designed to determine the 11 metal elements (Al, Cr, Mn, Fe, As, Ni, Cu, Zn, Cd, Sb, and Pb) in soy sauce and their migration from the containing glass bottles. Inductively coupled plasma mass spectrometry (ICP-MS) was applied for the determination of the elements and one-factor-at-a-time method was employed for optimizing the ICP-MS parameters in migration experiment and microwave digestion experiment. The developed method was successfully applied to determine the content of 11 elements. The results showed that the experiment had excellent correlation and sensitivity. The accuracy of the elements in the migration study and test of soy sauce itself ranging from 84.25% to 118.75% was satisfied, and the precision of the method was validated and the RSD was no more than 15.5%. The concentration of all the detected metal elements migrated from the glass bottles were between 0.3450 and 2.398 ng·mL−1, and the risk assessment indicated that the metal elements in soy sauce had no risk to the public health. The proposed methodology in this study was successfully applied for the quality control for metal elements in soy sauce and the containing glass bottles for the first time, and a research method suitable for soy sauce consumption process control and risk assessment has been established.
{"title":"One-factor-at-a-time method combined with ICP-MS for determining 11 elements in soy sauce and their migration from the containing glass bottles","authors":"Xun Gao, Kexin Chen, Yue Zhang, Miaomiao Chi","doi":"10.1515/revac-2022-0031","DOIUrl":"https://doi.org/10.1515/revac-2022-0031","url":null,"abstract":"Abstract This study was designed to determine the 11 metal elements (Al, Cr, Mn, Fe, As, Ni, Cu, Zn, Cd, Sb, and Pb) in soy sauce and their migration from the containing glass bottles. Inductively coupled plasma mass spectrometry (ICP-MS) was applied for the determination of the elements and one-factor-at-a-time method was employed for optimizing the ICP-MS parameters in migration experiment and microwave digestion experiment. The developed method was successfully applied to determine the content of 11 elements. The results showed that the experiment had excellent correlation and sensitivity. The accuracy of the elements in the migration study and test of soy sauce itself ranging from 84.25% to 118.75% was satisfied, and the precision of the method was validated and the RSD was no more than 15.5%. The concentration of all the detected metal elements migrated from the glass bottles were between 0.3450 and 2.398 ng·mL−1, and the risk assessment indicated that the metal elements in soy sauce had no risk to the public health. The proposed methodology in this study was successfully applied for the quality control for metal elements in soy sauce and the containing glass bottles for the first time, and a research method suitable for soy sauce consumption process control and risk assessment has been established.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"11 1","pages":"10 - 20"},"PeriodicalIF":4.3,"publicationDate":"2021-12-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86724891","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Porous graphitic carbon (PGC) is a widely used stationary phase for reversed-phase high-performance liquid chromatography (HPLC) that allows separation of structurally similar compounds retained in mixed form on a flat graphite surface. Such a stationary phase can be used in analytical chemistry to provide good separation and selectivity in pesticide monitoring. In this article, we studied the chromatographic behavior of five common triazine herbicides (simazine, atrazine, desmetryn, propazine, prometryn) on PGC vis-à-vis octadecyl-functionalized silica gel (ODS). It was found that the herbicides studied have an abnormal elution order on PGC compared to ODS. PGC was also characterized by higher selectivity of analyte separation. This behavior of triazine herbicides on PGC cannot be explained either with the help of existing theory or by mathematical modeling of adsorption processes on graphite. Therefore, we have proposed a possible retention mechanism, explaining the effects observed, due to the shielding of the amino group in the triazine ring by alkyl substituents, which decreases the “polar retention effect” of PGC. Satisfactory separation efficacy was obtained with the proposed analytical method, using convenient UV-detection and without resort to laborious techniques such as HPLC coupled with mass spectrometry.
{"title":"Abnormal retention of s-triazine herbicides on porous graphitic carbon","authors":"Oksana I. Grinevich, Z. Khesina, A. Buryak","doi":"10.1515/revac-2022-0029","DOIUrl":"https://doi.org/10.1515/revac-2022-0029","url":null,"abstract":"Abstract Porous graphitic carbon (PGC) is a widely used stationary phase for reversed-phase high-performance liquid chromatography (HPLC) that allows separation of structurally similar compounds retained in mixed form on a flat graphite surface. Such a stationary phase can be used in analytical chemistry to provide good separation and selectivity in pesticide monitoring. In this article, we studied the chromatographic behavior of five common triazine herbicides (simazine, atrazine, desmetryn, propazine, prometryn) on PGC vis-à-vis octadecyl-functionalized silica gel (ODS). It was found that the herbicides studied have an abnormal elution order on PGC compared to ODS. PGC was also characterized by higher selectivity of analyte separation. This behavior of triazine herbicides on PGC cannot be explained either with the help of existing theory or by mathematical modeling of adsorption processes on graphite. Therefore, we have proposed a possible retention mechanism, explaining the effects observed, due to the shielding of the amino group in the triazine ring by alkyl substituents, which decreases the “polar retention effect” of PGC. Satisfactory separation efficacy was obtained with the proposed analytical method, using convenient UV-detection and without resort to laborious techniques such as HPLC coupled with mass spectrometry.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"111 1","pages":"1 - 9"},"PeriodicalIF":4.3,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80579995","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
G. D’Orazio, C. Fanali, Chiara Dal Bosco, A. Gentili, S. Fanali
Abstract The determination and separation of enantiomers is an interesting and important topic of research in various fields, e.g., biochemistry, food science, pharmaceutical industry, environment, etc. Although these compounds possess identical physicochemical properties, a pair of enantiomers often has different pharmacological, toxicological, and metabolic activities. For this reason, chiral discrimination by using chromatographic and electromigration techniques has become an urgent need in the pharmaceutical field. This review intends to offer the “state of the art” about the separation of chiral antifungal drugs and several related precursors by both liquid and gas chromatography, as well as electromigration methods. This overview is organized into two sections. The first one describes general considerations on chiral antifungal drugs. The second part deals with the main analytical methods for the enantiomeric discrimination of these drugs, including a brief description of chiral selectors and stationary phases. Moreover, many recent applications attesting the great interest of analytical chemists in the field of enantiomeric separation are presented.
{"title":"Chiral separation and analysis of antifungal drugs by chromatographic and electromigration techniques: Results achieved in 2010–2020","authors":"G. D’Orazio, C. Fanali, Chiara Dal Bosco, A. Gentili, S. Fanali","doi":"10.1515/revac-2021-0136","DOIUrl":"https://doi.org/10.1515/revac-2021-0136","url":null,"abstract":"Abstract The determination and separation of enantiomers is an interesting and important topic of research in various fields, e.g., biochemistry, food science, pharmaceutical industry, environment, etc. Although these compounds possess identical physicochemical properties, a pair of enantiomers often has different pharmacological, toxicological, and metabolic activities. For this reason, chiral discrimination by using chromatographic and electromigration techniques has become an urgent need in the pharmaceutical field. This review intends to offer the “state of the art” about the separation of chiral antifungal drugs and several related precursors by both liquid and gas chromatography, as well as electromigration methods. This overview is organized into two sections. The first one describes general considerations on chiral antifungal drugs. The second part deals with the main analytical methods for the enantiomeric discrimination of these drugs, including a brief description of chiral selectors and stationary phases. Moreover, many recent applications attesting the great interest of analytical chemists in the field of enantiomeric separation are presented.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"50 1","pages":"220 - 252"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76672702","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract A new organic molecule probe has been introduced as a “turn-off” fluorescent sensor to detect trace quantities of UO2 2+ in the presence of several transition metals with promising results. The procedure is based on quenching the fluorescence intensity of 6-chloro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide (L) in the presence of various UO2 2+ concentrations in methanol. The UO2 2+ and L species interact through electrostatic interaction between negatively charged nitrogen atom of the sulfonamide group of L and positively charged UO2 2+, thus facilitating the non-radiative recombination of UO2 2+ and L through the charge transfer or electron transfer processes and leading to the fluorescence quenching of L. The mechanism of quenching was addressed and proved to be static quenching. The impressive quenching of the fluorescence intensity of L by different concentrations of UO2 2+ has been successfully used as a new sensor to measure UO2 2+ in methanol at λ ex = 340 nm, λ em = 380 nm with a linear dynamic range of 0.08–5.0 µM and detection limit and quantification limit of 0.0276 and 0.0837 µM, respectively. The L sensor shows interesting advantages compared to other developed sensors with adequate performance, such as broader linear range and lower detection limit, selectivity, and simplicity, which illustrate its useful practical use. Graphical abstract Fluorescence quenching detection of UO2 2+ in aqueous solution based on an organic molecule probe of 6-chloro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide.
{"title":"Fluorescence quenching detection of UO2 2+ in aqueous solution based on an organic molecule probe of 6-chloro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide","authors":"A. Elabd, O. A. Elhefnawy","doi":"10.1515/revac-2021-0123","DOIUrl":"https://doi.org/10.1515/revac-2021-0123","url":null,"abstract":"Abstract A new organic molecule probe has been introduced as a “turn-off” fluorescent sensor to detect trace quantities of UO2 2+ in the presence of several transition metals with promising results. The procedure is based on quenching the fluorescence intensity of 6-chloro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide (L) in the presence of various UO2 2+ concentrations in methanol. The UO2 2+ and L species interact through electrostatic interaction between negatively charged nitrogen atom of the sulfonamide group of L and positively charged UO2 2+, thus facilitating the non-radiative recombination of UO2 2+ and L through the charge transfer or electron transfer processes and leading to the fluorescence quenching of L. The mechanism of quenching was addressed and proved to be static quenching. The impressive quenching of the fluorescence intensity of L by different concentrations of UO2 2+ has been successfully used as a new sensor to measure UO2 2+ in methanol at λ ex = 340 nm, λ em = 380 nm with a linear dynamic range of 0.08–5.0 µM and detection limit and quantification limit of 0.0276 and 0.0837 µM, respectively. The L sensor shows interesting advantages compared to other developed sensors with adequate performance, such as broader linear range and lower detection limit, selectivity, and simplicity, which illustrate its useful practical use. Graphical abstract Fluorescence quenching detection of UO2 2+ in aqueous solution based on an organic molecule probe of 6-chloro-2H-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"58 1","pages":"136 - 143"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78859428","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Cilostazol (CLZ) is a quinolinone derivative possessing anti platelet and vasodilating properties and it is used in the treatment of intermittent claudication. It operates by inhibiting the cyclic guanosine monophosphate (cGMP) dependent phosphodiesterase III which leads to availability of cyclic adenosine monophosphate (cAMP) in blood vessels and platelets owing to vasodilation and reduced calcium-induced contractions. This article illustrates the various reported quantitative methods which can be used to determine cilostazol and its metabolites either alone or in combination forms in pharmaceutical preparation or biological matrices like plasma, serum, and urine. The review covers analytical methods like ultraviolet spectroscopy, fluorescence spectroscopy, electrometric methods, nuclear magnetic resonance spectroscopy, high performance liquid chromatography, high performance thin layer chromatography, ultra-high performance liquid chromatography, and tandem mass spectroscopy from the year 1985 to 2019 with a brief explanation on every analytical method. Among the methods, it was found that most researchers opted for UV and HPLC analytical methods for the estimation of cilostazol.
{"title":"An analytical review on the quantitative techniques for estimation of cilostazol in pharmaceutical preparations and biological samples","authors":"Afnaan Afreen, C. Nalini","doi":"10.1515/revac-2021-0128","DOIUrl":"https://doi.org/10.1515/revac-2021-0128","url":null,"abstract":"Abstract Cilostazol (CLZ) is a quinolinone derivative possessing anti platelet and vasodilating properties and it is used in the treatment of intermittent claudication. It operates by inhibiting the cyclic guanosine monophosphate (cGMP) dependent phosphodiesterase III which leads to availability of cyclic adenosine monophosphate (cAMP) in blood vessels and platelets owing to vasodilation and reduced calcium-induced contractions. This article illustrates the various reported quantitative methods which can be used to determine cilostazol and its metabolites either alone or in combination forms in pharmaceutical preparation or biological matrices like plasma, serum, and urine. The review covers analytical methods like ultraviolet spectroscopy, fluorescence spectroscopy, electrometric methods, nuclear magnetic resonance spectroscopy, high performance liquid chromatography, high performance thin layer chromatography, ultra-high performance liquid chromatography, and tandem mass spectroscopy from the year 1985 to 2019 with a brief explanation on every analytical method. Among the methods, it was found that most researchers opted for UV and HPLC analytical methods for the estimation of cilostazol.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"62 1","pages":"58 - 74"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83937450","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Allelopathy, a complex phenomenon has unveiled both stimulatory and inhibitory effects in plant processes that are mediated by the release of certain chemical compounds commonly known as allelochemicals. Allelochemicals, a form of bioactive secondary metabolites are produced by a diverse group of plants and microbes in response to biotic and abiotic stress. It ranges from a simple hydrocarbon to complex polycyclic aromatic compounds like phenol, flavonoids, tannins, steroids, amino acids, alkaloids and quinones. These plant bioactive compounds are released into the environment via decomposition, exudation, leaching and volatilization that play a significant role in regulating the intra-specific or inter-specific relations with counterparts. A wide variety of methods has been proposed for analyzing the basic mechanism and overall effect of allelochemicals. However, the lack of a reliable and effective method to identify their molecular mode of action and their modulation in the metabolic pathway still remains as a great challenge. From a commercial perspective, these allelochemicals are deemed to be better candidates for green natural herbicides and weedicides that are proven to be environment friendly, unlike synthetic chemicals. In order to pave a way for the economic viability of these chemicals, a basic understanding of their chemistry is inevitable. This review article is focused to give an in-depth understanding of metabolic pathways genes responsible for the elicitation/secretion and the adoption of a suitable downstream process and analytical techniques that can intensify the process.
{"title":"Synthesis and extraction routes of allelochemicals from plants and microbes: A review","authors":"A. Singh, G. Rajeswari, L. A. Nirmal, S. Jacob","doi":"10.1515/revac-2021-0139","DOIUrl":"https://doi.org/10.1515/revac-2021-0139","url":null,"abstract":"Abstract Allelopathy, a complex phenomenon has unveiled both stimulatory and inhibitory effects in plant processes that are mediated by the release of certain chemical compounds commonly known as allelochemicals. Allelochemicals, a form of bioactive secondary metabolites are produced by a diverse group of plants and microbes in response to biotic and abiotic stress. It ranges from a simple hydrocarbon to complex polycyclic aromatic compounds like phenol, flavonoids, tannins, steroids, amino acids, alkaloids and quinones. These plant bioactive compounds are released into the environment via decomposition, exudation, leaching and volatilization that play a significant role in regulating the intra-specific or inter-specific relations with counterparts. A wide variety of methods has been proposed for analyzing the basic mechanism and overall effect of allelochemicals. However, the lack of a reliable and effective method to identify their molecular mode of action and their modulation in the metabolic pathway still remains as a great challenge. From a commercial perspective, these allelochemicals are deemed to be better candidates for green natural herbicides and weedicides that are proven to be environment friendly, unlike synthetic chemicals. In order to pave a way for the economic viability of these chemicals, a basic understanding of their chemistry is inevitable. This review article is focused to give an in-depth understanding of metabolic pathways genes responsible for the elicitation/secretion and the adoption of a suitable downstream process and analytical techniques that can intensify the process.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"39 1","pages":"293 - 311"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73625127","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ivan Notardonato, Silvia Gianfagna, R. Castoria, G. Ianiri, F. De Curtis, M. V. Russo, P. Avino
Abstract This manuscript is a critical review of the analytical methods reported in the existing literature for the determination of mycotoxin patulin at trace/ultra-trace levels in food matrices. The article starts focusing on what mycotoxins are, their “analytical history” (more than 21,000 articles published in Scopus database): each mycotoxin is specific for a given fungus and shows toxic effects, some even being carcinogenic. Most International regulations on mycotoxins are also reported, which pertain official controls in the food chain as well as the sampling methods and the maximum tolerable limits of mycotoxins. Then the manuscript is focused on patulin, a mycotoxin that is mainly produced by the fungal species Penicillium expansum. The main characteristics and properties of patulin are discussed, including its biosynthesis, especially on stored fruits infected by P. expansum and derived products, its toxicology, and some strategies aiming at preventing and/or reducing its presence. The description of the analytical procedure for patulin starts from sampling: the extraction and analytical methods reported are based on the official protocol of the Association of Official Analytical Chemists, which relies on the high-performance liquid chromatography-ultraviolet/diode array detector (HPLC-UV/DAD). Furthermore, an in-depth discussion of the most suitable analytical methods is reported. The first analytical step regards the analyte(s) extraction from the sample, followed by a clean-up phase, and by a final quantitative determination. This last section is divided into reference or confirmation methods, rapid screening and new methods and expected results, i.e., qualitative, quantitative, or semi-quantitative. Reference methods include TLC, GC, HPLC, and MS, whereas rapid methods include enzyme immunoassay tests, dipsticks, and lateral flow tests. Novel analytical methods include fluorescence, near infrared spectroscopy, capillary electrophoresis, and biosensors. Finally, the official method is compared with others present in the literature allowing a multi-target analysis, and its use in combination with other techniques of molecularly imprinted polymers is discussed.
{"title":"Critical review of the analytical methods for determining the mycotoxin patulin in food matrices","authors":"Ivan Notardonato, Silvia Gianfagna, R. Castoria, G. Ianiri, F. De Curtis, M. V. Russo, P. Avino","doi":"10.1515/revac-2021-0131","DOIUrl":"https://doi.org/10.1515/revac-2021-0131","url":null,"abstract":"Abstract This manuscript is a critical review of the analytical methods reported in the existing literature for the determination of mycotoxin patulin at trace/ultra-trace levels in food matrices. The article starts focusing on what mycotoxins are, their “analytical history” (more than 21,000 articles published in Scopus database): each mycotoxin is specific for a given fungus and shows toxic effects, some even being carcinogenic. Most International regulations on mycotoxins are also reported, which pertain official controls in the food chain as well as the sampling methods and the maximum tolerable limits of mycotoxins. Then the manuscript is focused on patulin, a mycotoxin that is mainly produced by the fungal species Penicillium expansum. The main characteristics and properties of patulin are discussed, including its biosynthesis, especially on stored fruits infected by P. expansum and derived products, its toxicology, and some strategies aiming at preventing and/or reducing its presence. The description of the analytical procedure for patulin starts from sampling: the extraction and analytical methods reported are based on the official protocol of the Association of Official Analytical Chemists, which relies on the high-performance liquid chromatography-ultraviolet/diode array detector (HPLC-UV/DAD). Furthermore, an in-depth discussion of the most suitable analytical methods is reported. The first analytical step regards the analyte(s) extraction from the sample, followed by a clean-up phase, and by a final quantitative determination. This last section is divided into reference or confirmation methods, rapid screening and new methods and expected results, i.e., qualitative, quantitative, or semi-quantitative. Reference methods include TLC, GC, HPLC, and MS, whereas rapid methods include enzyme immunoassay tests, dipsticks, and lateral flow tests. Novel analytical methods include fluorescence, near infrared spectroscopy, capillary electrophoresis, and biosensors. Finally, the official method is compared with others present in the literature allowing a multi-target analysis, and its use in combination with other techniques of molecularly imprinted polymers is discussed.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"9 1","pages":"144 - 160"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84871694","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Francisco J. Espinosa, R. M. Toledano, J. Villén, J. M. Cortés, A. Vázquez
Abstract Large volume injection (LVI) in gas chromatography (GC) and online liquid chromatography-gas chromatography (LC-GC) are useful techniques for analyzing the compounds present at very low concentrations in complex samples since they substantially increase the sensitivity of the analysis and simplify sample preparation. LVI avoids the need to concentrate the extract and even the extraction step itself by directly injecting the sample. In online LC-GC, the liquid chromatography (LC) step acts as the sample preparation and/or fractionation step. The main problem in both techniques is the selective elimination of the large volume of solvent without losing the analytes. The TOTAD (through oven transfer adsorption–desorption) interface, based on a widely modified PTV (programmed temperature vaporizer) injector, allows large volumes to be injected into the gas chromatograph using both nonpolar and polar solvents, including water. Consequently, online LC-GC can be carried out whether the LC step is in the normal phase or the reversed phase. Various methods for analyzing trace compounds in food and environmental samples have been developed for LVI and online LC-GC using the TOTAD interface. Such analysis methods require the optimization of several variables common to LVI and online LC-GC and specific variables involved in online LC-GC, which must be optimized by taking into account the nature of the analytes and the characteristics of the sample matrix. This article reviews how each of these variables affects the performance of the analysis.
{"title":"TOTAD interface: A review of its application for LVI and LC-GC","authors":"Francisco J. Espinosa, R. M. Toledano, J. Villén, J. M. Cortés, A. Vázquez","doi":"10.1515/revac-2021-0138","DOIUrl":"https://doi.org/10.1515/revac-2021-0138","url":null,"abstract":"Abstract Large volume injection (LVI) in gas chromatography (GC) and online liquid chromatography-gas chromatography (LC-GC) are useful techniques for analyzing the compounds present at very low concentrations in complex samples since they substantially increase the sensitivity of the analysis and simplify sample preparation. LVI avoids the need to concentrate the extract and even the extraction step itself by directly injecting the sample. In online LC-GC, the liquid chromatography (LC) step acts as the sample preparation and/or fractionation step. The main problem in both techniques is the selective elimination of the large volume of solvent without losing the analytes. The TOTAD (through oven transfer adsorption–desorption) interface, based on a widely modified PTV (programmed temperature vaporizer) injector, allows large volumes to be injected into the gas chromatograph using both nonpolar and polar solvents, including water. Consequently, online LC-GC can be carried out whether the LC step is in the normal phase or the reversed phase. Various methods for analyzing trace compounds in food and environmental samples have been developed for LVI and online LC-GC using the TOTAD interface. Such analysis methods require the optimization of several variables common to LVI and online LC-GC and specific variables involved in online LC-GC, which must be optimized by taking into account the nature of the analytes and the characteristics of the sample matrix. This article reviews how each of these variables affects the performance of the analysis.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":"126 1","pages":"253 - 271"},"PeriodicalIF":4.3,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87736067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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