Chromatography (Basel)最新文献_第10页

Fluorous Derivatization Method for Selective Analysis of Curcumin with Liquid Chromatography-Tandem Mass Spectrometry 液相色谱-串联质谱法选择性分析姜黄素的氟衍生化方法

Chromatography (Basel) Pub Date : 2019-10-20 DOI: 10.15583/JPCHROM.2019.015

Shimba Kawasue, Yohei Sakaguchi, Ena Yano, Tadashi Hayama, Reiko Koga, H. Yoshida, H. Nohta

{"title":"Fluorous Derivatization Method for Selective Analysis of Curcumin with Liquid Chromatography-Tandem Mass Spectrometry","authors":"Shimba Kawasue, Yohei Sakaguchi, Ena Yano, Tadashi Hayama, Reiko Koga, H. Yoshida, H. Nohta","doi":"10.15583/JPCHROM.2019.015","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.015","url":null,"abstract":"Curcumin has been shown to be pharmacologically active in the prevention and treatment of various human diseases. In this study, we developed a fluorous derivatization method for selective analysis of curcumin with liquid chromatography (LC)tandem mass spectrometry (MS/MS). Curcumin was derivatized with the thiol-containing fluorous reagent (1H,1H,2H,2Hperfluoro-1-decanethiol) under mild conditions via Michael addition reaction, and the obtained derivative was introduced to a fluorous LC column (Fluofix-II 120E, 150 × 2.0 mm i.d., 5 μm, Wako). The selectively retained fluorous-derivatized curcumin on the column was also enabled highly sensitive detection with negative electrospray ionization MS/MS. Pretreatment of human serum sample was used protein precipitation with CH3CN. The calibration curve obtained by the present method showed good linearity (r2 = 0.9998) in the range of 7.4-442 ng/mL serum, and the limit of detection (S/N = 3) and limit of quantification (S/N = 10) were 1.8 ng/mL serum and 6.1 ng/mL serum, respectively. The present method was successfully applied to the analysis of curcumin in human serum sample.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/JPCHROM.2019.015","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43549500","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}

引用次数: 1

Dispersion of Graphene in an Aqueous Solution with Poly(sodium 4-styrenesulfonate) Monitored by Capillary Electrophoresis 用毛细管电泳监测石墨烯在聚（4-苯乙烯磺酸钠）水溶液中的分散

Chromatography (Basel) Pub Date : 2019-10-20 DOI: 10.15583/JPCHROM.2019.016

T. Takayanagi, Yuto Mizuta, Yuta Becchaku, H. Mizuguchi

{"title":"Dispersion of Graphene in an Aqueous Solution with Poly(sodium 4-styrenesulfonate) Monitored by Capillary Electrophoresis","authors":"T. Takayanagi, Yuto Mizuta, Yuta Becchaku, H. Mizuguchi","doi":"10.15583/JPCHROM.2019.016","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.016","url":null,"abstract":"Graphene was dispersed in an aqueous solution with poly(sodium 4-styrenesulfonate) as a dispersant. The charge of the graphene came to be apparently negative by the adsorption of poly(4-styrenesulfonate) ion (PSS). Two kinds of PSS were examined: the average molecular masses of 70,000 and 1,000,000 (PSS 70,000 and PSS 1,000,000, respectively). Capillary electrophoresis was used to evaluate the dispersion of the apparently anionic graphene in an aqueous solution. A broad signal corresponding to the dispersed graphene was detected in the electropherograms. The effective electrophoretic mobility of the dispersed graphene was somewhat larger at higher concentrations of PSS 70,000, suggesting that the adsorbed amount of PSS 70,000 increased. Even when the separation buffer did not contain PSS, the broad signal of the anionic graphene was still detected. The peak height and/or the peak area, as well as the effective electrophoretic mobility of the graphene decreased little at the reduced applied voltages, i.e., at longer separation/detection time. Therefore, the adsorption of PSS is irreversible or the desorption of PSS from the graphene surface is very slow. Accordingly, the dispersed graphene with PSS would be separated from the matrix PSS by the electrophoretic separation.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43460160","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}

引用次数: 1

Enantiomeric Separation of Chiral Alcohols Using Novel Core-Shell Type Chiral Stationary Phase Coated with Helical Poly(diphenylacetylene) Derivative by High-Performance Liquid Chromatography 螺旋聚二苯乙炔衍生物包被新型核-壳型手性固定相的高效液相色谱拆分手性醇对映体

Chromatography (Basel) Pub Date : 2019-10-20 DOI: 10.15583/jpchrom.2019.019

R. Nishioka, Syuji Harada, Kazuhiro Umehara

引用次数: 2

Fundamental Study of Behaviors of In-Source Collision Induced Dissociation and Shifting the Linear Range of Calibration Curves of Various Drugs and the Metabolites Used for Therapeutic Drug Monitoring 源内碰撞诱导解离行为的基础研究及用于治疗药物监测的各种药物和代谢物校准曲线线性范围的移动

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/jpchrom.2019.009

Masamitsu Maekawa, Taku Tsukamoto, Shinya Takasaki, M. Kikuchi, Yu Sato, Jiro Ogura, Yoshihiro Hayakawa, Hiroaki Yamaguchi, N. Mano

{"title":"Fundamental Study of Behaviors of In-Source Collision Induced Dissociation and Shifting the Linear Range of Calibration Curves of Various Drugs and the Metabolites Used for Therapeutic Drug Monitoring","authors":"Masamitsu Maekawa, Taku Tsukamoto, Shinya Takasaki, M. Kikuchi, Yu Sato, Jiro Ogura, Yoshihiro Hayakawa, Hiroaki Yamaguchi, N. Mano","doi":"10.15583/jpchrom.2019.009","DOIUrl":"https://doi.org/10.15583/jpchrom.2019.009","url":null,"abstract":"Therapeutic drug monitoring (TDM) is a clinical practice that designs personalized medication for patients with blood concentrations of the drug. TDM approach is used for many drugs, including immunosuppressant, antifungal, antiarrhythmic, and anti-cancer drugs. Combination therapies are often adopted in TDM. Liquid chromatography tandem mass spectrometry (LC-MS/MS) is a useful analytical method in such cases. However, the development of a simultaneous LC-MS/MS analytical method is difficult owing to the differences in MS sensitivity and the therapeutic range of each drug. In order to avoid saturation of the detector, in-source collision induced dissociation (CID) was used to reduce the ion inlet. In this study, we investigated the in-source CID behavior of 13 compounds of drugs and metabolites in TDM practice. As a result, all compounds provided a sharp reduction of ion inlet over the threshold ion guide voltage. In addition, a shift to the higher concentration of the calibration range was observed according to such changes. The intensity and linearity data in this study that all 13 drugs could be analyzed under in-source CID conditions simultaneously. These results might be useful for TDM of combination therapy in clinical practice.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/jpchrom.2019.009","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41262626","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}

引用次数: 3

LVSEP Analysis of Cationic Analytes in Non-Aqueous Capillary Electrophoresis 阳离子分析物在非水毛细管电泳中的LVSEP分析

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2019.008

F. Kitagawa, Osamu Osanai, Isoshi Nukatsuka

引用次数: 6

Selected Reaction Monitoring of Kinase Activity-Targeted Phosphopeptides 激酶活性靶向磷酸肽的选择性反应监测

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2019.005

Chisato Takahashi, Tatsuya Yazaki, Naoyuki Sugiyama, Y. Ishihama

{"title":"Selected Reaction Monitoring of Kinase Activity-Targeted Phosphopeptides","authors":"Chisato Takahashi, Tatsuya Yazaki, Naoyuki Sugiyama, Y. Ishihama","doi":"10.15583/JPCHROM.2019.005","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.005","url":null,"abstract":"We developed a capillary LC/MS/MS-based approach to monitor intracellular kinase activities. Selected reaction monitoring (SRM) mode was employed to quantitate a kinase substrate-digested peptide phosphorylated by kinase or kinase-digested peptides containing phosphosites which regulate the kinase activities. Ten kinases in EGFR-MAPK signaling pathway were targeted for the SRM assay and the experimental conditions such as the selection of target phosphopeptides, SRM transitions, LC parameters and sample pre-treatment steps were optimized. The validation study on accuracy, precision, linearity, limit of detection and limit of quantitation was carried out to confirm the capability for measuring the kinase activities through the phosphopeptide quantities in the biological samples. Finally, we applied this SRM assay to kinase activation dynamics induced by pervanadate, a tyrosine phosphatase inhibitor, in HeLa cells. As a result, it was found that 6 kinases out of 10 were activated, which were consistent with those by conventional Western blotting using phosphosite-specific antibodies. Since this SRM assay can be extended to kinome-wide analysis, it will be useful to unveil the entire signaling network in cells.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44230758","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}

引用次数: 3

Simultaneous Assay of Fecal Short-Chain Fatty and Bile Acids and Ratio of Total Bile Acids to Butyrate in Colon Cancer 结肠癌患者粪便短链脂肪、胆汁酸及总胆汁酸/丁酸比值的同时测定

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2018.022

T. Torii, K. Kanemitsu, A. Hagiwara

{"title":"Simultaneous Assay of Fecal Short-Chain Fatty and Bile Acids and Ratio of Total Bile Acids to Butyrate in Colon Cancer","authors":"T. Torii, K. Kanemitsu, A. Hagiwara","doi":"10.15583/JPCHROM.2018.022","DOIUrl":"https://doi.org/10.15583/JPCHROM.2018.022","url":null,"abstract":"We simultaneously quantified fecal bile acids (BAs) and short-chain fatty acids (SCFAs) florescence labeled with 9chloromethylanthracene using high-performance liquid chromatography-fluorescence (HPLC-FL) and developed an inexpensive and highly accurate method for determining the ratio of BAs and SCFAs in colorectal cancer patients and healthy controls. Samples were extracted with hexane/ether, and extractants were measured using HPLC-FL. The healthy subject group included 17 men and 21 women, whereas the colorectal cancer group included patients with cancer in the rectum (3 men, 2 women), sigmoid colon (3 men, 2 women), and ascending colon (2 men, 3 women). The contribution rate of determination for calibration curves was >0.99, and the additional recovery rate was 67.2%–107% for the simultaneous quantification of fecal BAs and SCFAs using HPLC-FL. Intra-day and inter-day variations in the control feces ranged 2.4%–5.1% and 3.1%–9.2%, respectively. The proportion of primary BAs to total BAs was higher in the colorectal cancer group (87.3%) than in the healthy subject group (67.9%). A significant difference was observed in the ratio of BAs to butyric acid between healthy subject and colorectal cancer groups. BA levels were higher in the colorectal cancer group. Thus, the ratio of total BAs to butyric acid may be a better predictor of colon cancer than BAs or SCFAs alone.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/JPCHROM.2018.022","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42757769","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}

引用次数: 3

Evaluation of the Interactions Between Palladium(II) and N,N’-Dimethyl-N,N’-di-n-hexyl-thiodiglycolamide in the Presence of Surfactants Using Capillary Electrophoresis 用毛细管电泳评价表面活性剂存在下钯（II）和N，N'-二甲基-N，N'--二正己基-硫代二甘醇酰胺之间的相互作用

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2019.007

Nana Tanaka, S. Kitagawa, H. Ohtani, Y. Iwama, K. Kondo, Yuzo Ishigaki, N. Shibata, T. Kinoshita, Y. Kamimoto, R. Ichino

{"title":"Evaluation of the Interactions Between Palladium(II) and N,N’-Dimethyl-N,N’-di-n-hexyl-thiodiglycolamide in the Presence of Surfactants Using Capillary Electrophoresis","authors":"Nana Tanaka, S. Kitagawa, H. Ohtani, Y. Iwama, K. Kondo, Yuzo Ishigaki, N. Shibata, T. Kinoshita, Y. Kamimoto, R. Ichino","doi":"10.15583/JPCHROM.2019.007","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.007","url":null,"abstract":"Continuous counter-current foam separation (CCFS) is a method for the recovery of valuable metals with high selectivity. It was developed as an organic solvent-free method, and the interaction of surfactants and metal ions in aqueous solution is a key precondition for the successful recovery. In this study, the interactions between the anionic complex of palladium(II) chloride and N , N ’-dimethyl- N , N ’-di- n -hexyl-thiodiglycolamide (MHTDA), which is an extraction agent for palladium(II), were investigated by capillary electrophoresis, in the presence of surfactants (sodium dodecyl sulfate (SDS) or polyoxyethylene mono-4-octylphenyl ether (POOPE)). The addition of MHTDA to an electrophoretic media containing SDS, resulted in electropherograms composed of two or three peaks. On the other hand, in the case of an electrophoretic media containing POOPE, the elimination of palladium (II) peak was observed due to MHTDA addition. This behavior suggested that the palladium-MHTDA neutral complex is rapidly captured in the POOPE micelles compared with the SDS micelles, and the use of POOPE is effective for the successful recovery of palladium(II) in CCFS.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42802091","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}

引用次数: 2

Analysis of 2-Aminobenzoic Acid-Labeled Monosaccharides and Glycoprotein-Derived Oligosaccharides by Online Cleanup Liquid Chromatography in the Reversed-Phase and Hydrophilic Interaction Liquid Chromatography Modes 反相和亲水相互作用液相色谱法在线清除液相色谱分析2-氨基苯甲酸标记的单糖和糖蛋白衍生的低聚糖

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2019.006

Sachio Yamamoto, Yuki Hayashi, H. Matsunaga, Fuka Okada, M. Kinoshita, Shigeo Suzuki

{"title":"Analysis of 2-Aminobenzoic Acid-Labeled Monosaccharides and Glycoprotein-Derived Oligosaccharides by Online Cleanup Liquid Chromatography in the Reversed-Phase and Hydrophilic Interaction Liquid Chromatography Modes","authors":"Sachio Yamamoto, Yuki Hayashi, H. Matsunaga, Fuka Okada, M. Kinoshita, Shigeo Suzuki","doi":"10.15583/JPCHROM.2019.006","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.006","url":null,"abstract":"Quantitative analysis of monosaccharides or glycoprotein glycans by high-performance liquid chromatography (HPLC) often involves labeling of the saccharide aldehyde groups with fluorescent tags to enhance sensitivity and selectivity. However, the methods required to remove the large excess of labeling reagents from the reaction mixture are time-consuming. Furthermore, these methods often hinder the quantitative analysis of the labeled samples. Here, we developed an online sample cleanup procedure for HPLC analysis of 2-aminobenzoic acid (2-AA)-labeled monosaccharides or oligosaccharides using a ten-port valve and mini columns. An online purification system using a combination of short HLB columns with the valve was proposed for the analysis of 2-AA-labeled monosaccharides utilizing reversed-phase modes. In the analysis of 2-AA-labeled glycans derived from glycoproteins, a short CN column with the valve was proposed utilizing hydrophilic interaction liquid chromatography (HILIC) modes. Optimized conditions enabled the direct injection of the diluted labeling reaction mixture into the chromatographic system without any prior removal of the excess labeling reagents. These methods were successfully applied to the analysis of various monosaccharides and N -linked glycans released from specific glycoproteins.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/JPCHROM.2019.006","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44171981","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}

引用次数: 1

Determination of Chiral Amino Acids in Various Fermented Products Using a Two-Dimensional HPLC-MS/MS System 二维HPLC-MS/MS系统测定各种发酵产物中的手性氨基酸

Chromatography (Basel) Pub Date : 2019-06-20 DOI: 10.15583/JPCHROM.2019.011

Chiharu Ishii, T. Akita, M. Nagano, M. Mita, K. Hamase

{"title":"Determination of Chiral Amino Acids in Various Fermented Products Using a Two-Dimensional HPLC-MS/MS System","authors":"Chiharu Ishii, T. Akita, M. Nagano, M. Mita, K. Hamase","doi":"10.15583/JPCHROM.2019.011","DOIUrl":"https://doi.org/10.15583/JPCHROM.2019.011","url":null,"abstract":"Chiral amino acids in fermented products including Japanese traditional black vinegar, a processed cheese and nam pla were determined using an on-line two-dimensional (2D) HPLC-MS/MS system. As the target amino acids, Ala, Asp, Glu, Leu, Pro and Ser were selected. Prior to the HPLC separation, the fermented products were appropriately homogenized and deproteinized, then amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F). Using the 2D-HPLC system, the target NBD-amino acids were individually purified by a microbore reversed-phase column in the first dimension and further separated by a narrowbore enantioselective column in the second dimension. The detection was performed by a fluorescence detector and also by a tandem mass spectrometer. Compared to the 2D-HPLC with fluorescence detection, the target chiral amino acids in complicated real world matrices were successfully determined using the 2D HPLC-MS/MS system without interference by the co-elution of unknown intrinsic compounds. In all the tested fermented products, various D-amino acids were observed, and the obtained values were 0.02-6.21 mmol/L (%D=0.7-29.2%) in the black vinegar, 0.02-0.73 μmol/g (0.2-24.8%) in the processed cheese and 0.07-2.30 mmol/L (0.5-23.5%) in the nam pla.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/JPCHROM.2019.011","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49344896","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}

引用次数: 9