It is essential to monitor pesticides in soils as their presence at trace levels and their bioavailability can induce adverse effects on soil's ecosystems, animals, and human health. In this study, we developed an analytical method for the quantification of traces of multi-class pesticides in soil using liquid chromatography-tandem mass spectrometry. In this way, 31 pesticides were selected, including 12 herbicides, 9 insecticides, and 10 fungicides. Two extraction techniques were first evaluated, namely, the pressurized liquid extraction and the QuEChERS procedure. The latest one was finally selected and optimized, allowing extraction recoveries of 55 to 118%. The role of the chelating agent EDTA, which binds preferentially to soil cations that complex some pesticides, was highlighted. Coupled with liquid chromatography-tandem mass spectrometry, the procedure displayed very high sensitivity, with limits of quantification (LOQ) in the range 0.01-5.5 ng/g. A good linearity (R2 > 0.992) was observed over two orders of magnitude (LOQ-100 [Formula: see text] LOQ) with good accuracy (80-120%) for all compounds except the two pyrethroids lambda-cyhalothrin and tau-fluvalinate (accuracy comprised between 50 and 175%) and the cyclohexanedione cycloxydim (accuracy < 35%). Good repeatability and reproducibility were also achieved. The method was finally successfully applied to 12 soil samples collected from 3 land-use types. Among the 31-targeted pesticides, 24 were detected at least once, with concentration levels varying from LOQ to 722 ng/g. Many values were below 0.5 ng/g, indicating that the developed method could provide new knowledge on the extremely low residual contents of some pesticides.
{"title":"Ultrasound-assisted QuEChERS-based extraction using EDTA for determination of currently-used pesticides at trace levels in soil.","authors":"Florent Lafay, Gaëlle Daniele, Maëva Fieu, Céline Pelosi, Clémentine Fritsch, Emmanuelle Vulliet","doi":"10.1007/s11356-022-19397-3","DOIUrl":"10.1007/s11356-022-19397-3","url":null,"abstract":"<p><p>It is essential to monitor pesticides in soils as their presence at trace levels and their bioavailability can induce adverse effects on soil's ecosystems, animals, and human health. In this study, we developed an analytical method for the quantification of traces of multi-class pesticides in soil using liquid chromatography-tandem mass spectrometry. In this way, 31 pesticides were selected, including 12 herbicides, 9 insecticides, and 10 fungicides. Two extraction techniques were first evaluated, namely, the pressurized liquid extraction and the QuEChERS procedure. The latest one was finally selected and optimized, allowing extraction recoveries of 55 to 118%. The role of the chelating agent EDTA, which binds preferentially to soil cations that complex some pesticides, was highlighted. Coupled with liquid chromatography-tandem mass spectrometry, the procedure displayed very high sensitivity, with limits of quantification (LOQ) in the range 0.01-5.5 ng/g. A good linearity (R<sup>2</sup> > 0.992) was observed over two orders of magnitude (LOQ-100 [Formula: see text] LOQ) with good accuracy (80-120%) for all compounds except the two pyrethroids lambda-cyhalothrin and tau-fluvalinate (accuracy comprised between 50 and 175%) and the cyclohexanedione cycloxydim (accuracy < 35%). Good repeatability and reproducibility were also achieved. The method was finally successfully applied to 12 soil samples collected from 3 land-use types. Among the 31-targeted pesticides, 24 were detected at least once, with concentration levels varying from LOQ to 722 ng/g. Many values were below 0.5 ng/g, indicating that the developed method could provide new knowledge on the extremely low residual contents of some pesticides.</p>","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"37 1","pages":""},"PeriodicalIF":5.8,"publicationDate":"2022-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89215840","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 : 2022-02-04DOI: 10.15583/jpchrom.2021.021
Eisuke Kanao
π interactions have recently received considerable attentions due to principal factor governing molecular recognitions and self-assemble abilities, as accumulated in the database on proximate arrangements in structures of biological systems and organic functional materials. Therefore, further deep understanding and control of π interactions will greatly facilitate the development of new functional materials. Despite the importance of π interactions, they are still challenging to study because π interactions are much weaker than most other molecular interactions, such as hydrophobic interaction, hydrogen bonding, and electrostatic bonding. On the other hand, liquid chromatography (LC) is a powerful separation technique, which is able to distinguish the partition coefficients of solutes between the mobile and stationary phases, and can sensitively reflect the strength of molecular interactions. We investigated the properties of π interactions by developing new silica-monolithic capillary columns modified with carbon materials providing strong π interactions. In this focusing review, we introduce a few specific π interactions by columns modified with fullerenes and polycyclic aromatic hydrocarbons (PAHs), which showed strong π - π interactions due to spherical recognition and multiple CH- π interactions. Furthermore, π interactions can contribute to the separation of various samples, which are difficult to achieve by the available retention mechanisms. Briefly, we applied various π interactions to specific separation analyses, and we succeeded in separating halogenated compounds, H/D isotopologue pairs, and saccharides by effective π interactions. These results indicates that π interactions contribute to practical separation science, such as removal of environmental pollutants and quantitative determination of medicinal compounds.
{"title":"Studies on π Interactions in Liquid-phase Separations","authors":"Eisuke Kanao","doi":"10.15583/jpchrom.2021.021","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.021","url":null,"abstract":"π interactions have recently received considerable attentions due to principal factor governing molecular recognitions and self-assemble abilities, as accumulated in the database on proximate arrangements in structures of biological systems and organic functional materials. Therefore, further deep understanding and control of π interactions will greatly facilitate the development of new functional materials. Despite the importance of π interactions, they are still challenging to study because π interactions are much weaker than most other molecular interactions, such as hydrophobic interaction, hydrogen bonding, and electrostatic bonding. On the other hand, liquid chromatography (LC) is a powerful separation technique, which is able to distinguish the partition coefficients of solutes between the mobile and stationary phases, and can sensitively reflect the strength of molecular interactions. We investigated the properties of π interactions by developing new silica-monolithic capillary columns modified with carbon materials providing strong π interactions. In this focusing review, we introduce a few specific π interactions by columns modified with fullerenes and polycyclic aromatic hydrocarbons (PAHs), which showed strong π - π interactions due to spherical recognition and multiple CH- π interactions. Furthermore, π interactions can contribute to the separation of various samples, which are difficult to achieve by the available retention mechanisms. Briefly, we applied various π interactions to specific separation analyses, and we succeeded in separating halogenated compounds, H/D isotopologue pairs, and saccharides by effective π interactions. These results indicates that π interactions contribute to practical separation science, such as removal of environmental pollutants and quantitative determination of medicinal compounds.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47397186","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 : 2022-02-03DOI: 10.15583/jpchrom.2022.001
Ohjiro Sumiya, Koki Nakagami, I. Ueta, Yoshihiro Saito
A novel spherical polymeric material has been introduced as a stationary phase in liquid chromatography (LC). Poly(benzoguanamine- co -melamine- co -formaldehyde) (BMF) was packed into a stainless-steel tube having 4.6 mm i.d., 150 mm length, as a particulate separation medium in LC. The retention behavior for polycyclic aromatic compounds (PACs) on the BMF phase was evaluated in reversed-phase LC and the trend was compared with that on a commercially-available octadecylsilica (ODS) phase. The BMF phase showed a unique molecular shape selectivity for PACs that was clearly different from that on typical ODS phases. The BMF stationary phase more strongly retained "rod-like" molecules such as naphthacene than "square-like" molecules with a relatively large molecular weight. From the results, it was considered that the phenyl groups as stationary phase ligands were exposed on the surface of BMF particles, and these phenyl functionalities were apart from each other. Therefore, the BMF phase strongly retained "rod-like" analyte molecules that can interact with more than one phenyl groups simultaneously of the stationary phase.
{"title":"Molecular Shape Selectivity for Polycyclic Aromatic Compounds on a Poly(benzoguanamine-co-melamine-co-formaldehyde) Stationary Phase in Reversed-Phase Liquid Chromatography","authors":"Ohjiro Sumiya, Koki Nakagami, I. Ueta, Yoshihiro Saito","doi":"10.15583/jpchrom.2022.001","DOIUrl":"https://doi.org/10.15583/jpchrom.2022.001","url":null,"abstract":"A novel spherical polymeric material has been introduced as a stationary phase in liquid chromatography (LC). Poly(benzoguanamine- co -melamine- co -formaldehyde) (BMF) was packed into a stainless-steel tube having 4.6 mm i.d., 150 mm length, as a particulate separation medium in LC. The retention behavior for polycyclic aromatic compounds (PACs) on the BMF phase was evaluated in reversed-phase LC and the trend was compared with that on a commercially-available octadecylsilica (ODS) phase. The BMF phase showed a unique molecular shape selectivity for PACs that was clearly different from that on typical ODS phases. The BMF stationary phase more strongly retained \"rod-like\" molecules such as naphthacene than \"square-like\" molecules with a relatively large molecular weight. From the results, it was considered that the phenyl groups as stationary phase ligands were exposed on the surface of BMF particles, and these phenyl functionalities were apart from each other. Therefore, the BMF phase strongly retained \"rod-like\" analyte molecules that can interact with more than one phenyl groups simultaneously of the stationary phase.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49258823","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 : 2022-01-20DOI: 10.15583/jpchrom.2021.022
T. Takayanagi
Electrophoretic migration of an analyte in capillary electrophoresis (CE) reflects reaction dynamics of the analyte in solution. In affinity CE, an analyte of interest interacts with a modifier added in the separation buffer in fast equilibrium, and effective electrophoretic mobility of the analyte is contributed from its equilibrium species. Precise measurement of effective electrophoretic mobility allows analyzing the equilibrium. Analysis of equilibria under CE separation possesses several advantages against traditional analyses in homogeneous solution; coexisting substances including impurities and kinetically generated substances are resolved by CE from the equilibrium species of interest. Characteristics of the CE analysis have been applied to analyses of acid-base equilibria of degradable substances and ion-association equilibria in an aqueous solution. Since CE is operated in an open-tubular capillary, it is also suitable for the characterization of carbon nanoclusters such as graphene and carbon nanotube, and measurement of effective electrophoretic mobility helps characterization of nanoclusters. A novel analysis technique of capillary electrophoresis/dynamic frontal analysis (CE/DFA) has also been proposed for the analysis of such reactions as involving equilibria and kinetic reactions. In CE/DFA, kinetically generated product is continuously resolved from the equilibrium species, and a plateau signal would be detected when the reaction rate is constant. Michaelis-Menten constants have successfully been determined through the plateau height by CE/DFA. In this review, analysis and characterization methods utilizing reaction dynamics in a separation capillary are summarized.
{"title":"Development of Novel Analysis and Characterization Methods Utilizing Reaction Dynamics in a Separation Capillary","authors":"T. Takayanagi","doi":"10.15583/jpchrom.2021.022","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.022","url":null,"abstract":"Electrophoretic migration of an analyte in capillary electrophoresis (CE) reflects reaction dynamics of the analyte in solution. In affinity CE, an analyte of interest interacts with a modifier added in the separation buffer in fast equilibrium, and effective electrophoretic mobility of the analyte is contributed from its equilibrium species. Precise measurement of effective electrophoretic mobility allows analyzing the equilibrium. Analysis of equilibria under CE separation possesses several advantages against traditional analyses in homogeneous solution; coexisting substances including impurities and kinetically generated substances are resolved by CE from the equilibrium species of interest. Characteristics of the CE analysis have been applied to analyses of acid-base equilibria of degradable substances and ion-association equilibria in an aqueous solution. Since CE is operated in an open-tubular capillary, it is also suitable for the characterization of carbon nanoclusters such as graphene and carbon nanotube, and measurement of effective electrophoretic mobility helps characterization of nanoclusters. A novel analysis technique of capillary electrophoresis/dynamic frontal analysis (CE/DFA) has also been proposed for the analysis of such reactions as involving equilibria and kinetic reactions. In CE/DFA, kinetically generated product is continuously resolved from the equilibrium species, and a plateau signal would be detected when the reaction rate is constant. Michaelis-Menten constants have successfully been determined through the plateau height by CE/DFA. In this review, analysis and characterization methods utilizing reaction dynamics in a separation capillary are summarized.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43045053","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 : 2022-01-15DOI: 10.15583/jpchrom.2021.020
Aogu Furusho, Karina Akemy IKEJIRI, Chiharu Ishii, T. Akita, M. Mita, M. Nagano, T. Ide, K. Hamase
A two-dimensional high-performance liquid chromatographic (2D-HPLC) system using the pre-column derivatization with 4-( N , N -dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F) has been developed for the determination of alanine (Ala), aspartic acid (Asp) and serine (Ser) enantiomers. For the precise determination of trace amounts of D -amino acids in complex matrices, a highly sensitive and selective method is required. In the present study, amino acids were derivatized with DBD-F for the sensitive fluorescence detection and were analyzed by a selective 2D-HPLC system combining a reversed-phase column (Singularity RP18, 1.0 x 500 mm) and an enantioselective column (Singularity CSP-001S, 1.5 x 250 mm). The established system was successfully applied to the chiral amino acid analyses of Japanese traditional amber rice vinegar, human plasma and human urine samples. In the Japanese traditional amber rice vinegar and human urine, relatively high amounts of all the target D -amino acids were observed (% D =5.8-37.7), while trace amounts of D -Ser and D -Ala were found in human plasma (% D =0.5-2.1).
建立了4-(N, N -二甲氨基磺酰基)-7-氟-2,1,3-苯并恶二唑(DBD-F)柱前衍生的二维高效液相色谱(2D-HPLC)体系，用于测定丙氨酸(Ala)、天冬氨酸(Asp)和丝氨酸(Ser)对映体。为了精确测定复杂基质中微量D -氨基酸，需要一种高灵敏度和选择性的方法。在本研究中，氨基酸被DBD-F衍生化以进行灵敏的荧光检测，并通过选择性2D-HPLC系统进行分析，该系统由反相柱(Singularity RP18, 1.0 x 500 mm)和对映选择性柱(Singularity CSP-001S, 1.5 x 250 mm)组成。建立的系统成功地应用于日本传统琥珀米醋、人血浆和人尿液样品的手性氨基酸分析。在日本传统琥珀米醋和人类尿液中，观察到所有目标D -氨基酸的含量相对较高(% D =5.8-37.7)，而在人类血浆中发现微量的D -Ser和D -Ala (% D =0.5-2.1)。
{"title":"Two-Dimensional High-Performance Liquid Chromatographic Determination of Chiral Amino Acids in Food Samples and Human Physiological Fluids Using Fluorescence Derivatization with 4-(N,N-Dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole","authors":"Aogu Furusho, Karina Akemy IKEJIRI, Chiharu Ishii, T. Akita, M. Mita, M. Nagano, T. Ide, K. Hamase","doi":"10.15583/jpchrom.2021.020","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.020","url":null,"abstract":"A two-dimensional high-performance liquid chromatographic (2D-HPLC) system using the pre-column derivatization with 4-( N , N -dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F) has been developed for the determination of alanine (Ala), aspartic acid (Asp) and serine (Ser) enantiomers. For the precise determination of trace amounts of D -amino acids in complex matrices, a highly sensitive and selective method is required. In the present study, amino acids were derivatized with DBD-F for the sensitive fluorescence detection and were analyzed by a selective 2D-HPLC system combining a reversed-phase column (Singularity RP18, 1.0 x 500 mm) and an enantioselective column (Singularity CSP-001S, 1.5 x 250 mm). The established system was successfully applied to the chiral amino acid analyses of Japanese traditional amber rice vinegar, human plasma and human urine samples. In the Japanese traditional amber rice vinegar and human urine, relatively high amounts of all the target D -amino acids were observed (% D =5.8-37.7), while trace amounts of D -Ser and D -Ala were found in human plasma (% D =0.5-2.1).","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46383748","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 : 2021-12-24DOI: 10.15583/jpchrom.2021.016
Takuma Ohtawa, M. Tsunoda
2-Hydroxyglutarate (2-HG) was enantiomerically separated using copper(II) acetate and N,N-dimethyl-L-phenylalanine as chiral additives. These compounds formed diastereomeric complexes with 2-HG, which were successfully separated on an achiral (ODS) column. Several parameters, such as additive concentration, the type of organic modifier, and column temperature, were optimized. Using the optimal mobile phase (1 mM copper(II) acetate and 2 mM N,N-dimethyl-L-phenylalanine in a 10% aqueous methanol solution), 2-HG enantiomers were successfully separated in 15 min with a resolution of 1.93.
{"title":"Enantiomeric Separation of 2-Hydroxyglutarate Using Chiral Mobile Phase Additives","authors":"Takuma Ohtawa, M. Tsunoda","doi":"10.15583/jpchrom.2021.016","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.016","url":null,"abstract":"2-Hydroxyglutarate (2-HG) was enantiomerically separated using copper(II) acetate and N,N-dimethyl-L-phenylalanine as chiral additives. These compounds formed diastereomeric complexes with 2-HG, which were successfully separated on an achiral (ODS) column. Several parameters, such as additive concentration, the type of organic modifier, and column temperature, were optimized. Using the optimal mobile phase (1 mM copper(II) acetate and 2 mM N,N-dimethyl-L-phenylalanine in a 10% aqueous methanol solution), 2-HG enantiomers were successfully separated in 15 min with a resolution of 1.93.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-12-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44970819","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 : 2021-12-10DOI: 10.15583/jpchrom.2021.019
Koichi Saito, Yukie Arima, Miho Morooka, Yoshiyuki Kobayashi, R. Ito
We elucidated factors for the chiral conversion of α -lipoic acid enantiomers in α -lipoic acid-containing dietary supplements. Samples were cleaned up by the solid-phase dispersive extraction method using Oasis MAX and MCX as the solid-phase gel. The α -lipoic acid enantiomers were reciprocally converted by heating at 180°C, and finally became a racemate. The chiral conversion rate changed depending on sample purity, particularly the presence or absence of coexisting components in the dietary supplements. As candidates for coexisting components, neutral nonionic and highly polar substances were suggested, such as sugars. We found that chiral conversion was promoted by heating in the presence of glucose. Oftentimes, a relatively large amount of S -(–)- α -lipoic acid is detected in dietary supplements claiming to contain R -(+)- α -lipoic acid on the bottle label. We speculate that the proportion of S -form may have been increased by coexisting components such as glucose when heat treatment is performed during the manufacturing process.
{"title":"Elucidation of Factors for Chiral Conversion of α-Lipoic Acid in Dietary Supplement","authors":"Koichi Saito, Yukie Arima, Miho Morooka, Yoshiyuki Kobayashi, R. Ito","doi":"10.15583/jpchrom.2021.019","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.019","url":null,"abstract":"We elucidated factors for the chiral conversion of α -lipoic acid enantiomers in α -lipoic acid-containing dietary supplements. Samples were cleaned up by the solid-phase dispersive extraction method using Oasis MAX and MCX as the solid-phase gel. The α -lipoic acid enantiomers were reciprocally converted by heating at 180°C, and finally became a racemate. The chiral conversion rate changed depending on sample purity, particularly the presence or absence of coexisting components in the dietary supplements. As candidates for coexisting components, neutral nonionic and highly polar substances were suggested, such as sugars. We found that chiral conversion was promoted by heating in the presence of glucose. Oftentimes, a relatively large amount of S -(–)- α -lipoic acid is detected in dietary supplements claiming to contain R -(+)- α -lipoic acid on the bottle label. We speculate that the proportion of S -form may have been increased by coexisting components such as glucose when heat treatment is performed during the manufacturing process.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46390114","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 : 2021-11-12DOI: 10.15583/jpchrom.2021.018
F. Kitagawa, Ayaka Hayashi, Isoshi Nukatsuka
To achieve highly sensitive analyses of phosphopeptides with simple experimental procedures in capillary electrophoresis (CE) and microchip electrophoresis (MCE), large-volume sample stacking with an electroosmotic flow pump (LVSEP) was performed in dynamically poly(vinyl pyrrolidone) (PVP)-coated capillaries to suppress the electroosmotic flow. In the analysis of monophosphopeptide (MPP) from bovine β -casein, good enrichments were attained with the sensitive enhancement factor (SEF) of 260 and 400 in CE and MCE, respectively, by using 0.2% PVP in 20 mM HEPES buffer (pH 9.0) in LVSEP.
为了在毛细管电泳(CE)和微芯片电泳(MCE)中实现高灵敏度的磷酸肽分析，采用电渗透泵(LVSEP)在聚乙烯吡罗烷酮(PVP)动态包被的毛细血管中进行大容量样品堆积，以抑制电渗透流动。在对牛β -酪蛋白单磷酸肽(MPP)的分析中，在20 mM HEPES缓冲液(pH 9.0)中使用0.2% PVP，在CE和MCE中分别以260和400的敏感增强因子(SEF)获得了较好的富集效果。
{"title":"LVSEP Analysis of Phosphopeptides in Dynamically PVP-Coated Capillaries and Microchannels","authors":"F. Kitagawa, Ayaka Hayashi, Isoshi Nukatsuka","doi":"10.15583/jpchrom.2021.018","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.018","url":null,"abstract":"To achieve highly sensitive analyses of phosphopeptides with simple experimental procedures in capillary electrophoresis (CE) and microchip electrophoresis (MCE), large-volume sample stacking with an electroosmotic flow pump (LVSEP) was performed in dynamically poly(vinyl pyrrolidone) (PVP)-coated capillaries to suppress the electroosmotic flow. In the analysis of monophosphopeptide (MPP) from bovine β -casein, good enrichments were attained with the sensitive enhancement factor (SEF) of 260 and 400 in CE and MCE, respectively, by using 0.2% PVP in 20 mM HEPES buffer (pH 9.0) in LVSEP.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42459437","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 : 2021-10-12DOI: 10.15583/jpchrom.2021.017
C. Hsieh, Chiharu Ishii, T. Akita, A. Fujii, Kazunori Hashiguchi, M. Nagano, M. Mita, Jen-Ai Lee, K. Hamase
{"title":"Chiral Analysis of Lactate in Various Food Samples Including Japanese Traditional Amber Rice Vinegar and the Developmental Changes During Fermentation Processes","authors":"C. Hsieh, Chiharu Ishii, T. Akita, A. Fujii, Kazunori Hashiguchi, M. Nagano, M. Mita, Jen-Ai Lee, K. Hamase","doi":"10.15583/jpchrom.2021.017","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.017","url":null,"abstract":"","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46763529","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 : 2021-10-10DOI: 10.15583/jpchrom.2021.012
Natsuki Iwata, Y. Watabe, Shin Horie, Yoshihiro Hayakawa
{"title":"A Novel Determination Method of Thirty-Seven o-Phthalaldehyde-Derivatized D/L-Amino Acids with Complementary Use of Two Chiral Thiols by High Performance Liquid Chromatography","authors":"Natsuki Iwata, Y. Watabe, Shin Horie, Yoshihiro Hayakawa","doi":"10.15583/jpchrom.2021.012","DOIUrl":"https://doi.org/10.15583/jpchrom.2021.012","url":null,"abstract":"","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46070685","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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