ChromatographyPub Date : 2023-10-20DOI: 10.15583/jpchrom.2023.014
Ikuo UETA, Hiroto MAKABE, Suguru MASUDA, Koki NAKAGAMI, Yoshihiro SAITO
{"title":"Foam-Eliminatory Purge-and-Trap Technique Using a Functional PTFE Membrane and Needle-Type Extraction Device to Determine Flavors in Drink Samples","authors":"Ikuo UETA, Hiroto MAKABE, Suguru MASUDA, Koki NAKAGAMI, Yoshihiro SAITO","doi":"10.15583/jpchrom.2023.014","DOIUrl":"https://doi.org/10.15583/jpchrom.2023.014","url":null,"abstract":"A simple and sensitive method for determining flavor compounds in foamable liquid samples was developed using the purge-and-trap method with the addition of glass wool and a functional porous polytetrafluoroethylene (PTFE) membrane. Flavor compounds purged from sample solutions were trapped by a needle-type extraction device. The functional PTFE membrane, which retained the aqueous sample while allowing purge gas to pass, was fixed on a glass solid-phase extraction cartridge. Hence, purge gas was continuously introduced into the sample solution from the bottom of the cartridge. To trap the foam, 0.4 g of glass wool was fixed in the sample headspace, and headspace gas was collected using a needle-type extraction device placed on the upper side of the wool. During the purge process, although foam climbed through the cartridge, it was adsorbed on the glass wool. However, the flavor compounds were not adsorbed on the inactive glass wool surface as confirmed in this study. This method does not require the dilution of sample solutions or the adding of antifoam agents to sample solutions. This simple and inexpensive construction enables the sensitive detection of flavor compounds.","PeriodicalId":10272,"journal":{"name":"Chromatography","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135513646","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}
ChromatographyPub Date : 2023-10-20DOI: 10.15583/jpchrom.2023.017
Ikuo UETA, Syuhei KAMEI, Koki NAKAGAMI, Yoshihiro SAITO
{"title":"Determination of Volatile Polycyclic Aromatic Hydrocarbons in Soil Using Needle-Type Extraction","authors":"Ikuo UETA, Syuhei KAMEI, Koki NAKAGAMI, Yoshihiro SAITO","doi":"10.15583/jpchrom.2023.017","DOIUrl":"https://doi.org/10.15583/jpchrom.2023.017","url":null,"abstract":"A new analytical method for the quantification of volatile polycyclic aromatic hydrocarbons (PAHs) in soil samples using a needle-type extraction device was developed. Naphthalene (Nap), acenaphthylene (Acy), acenaphthene (Ace), and fluorene (Flu) were investigated as analytes. Samples were prepared by placing 10 g of soil in a glass cartridge and immersing the cartridge in a 75°C water bath. The needle-type extraction device packed with Carbopack X and carbon molecular sieve was inserted into the glass cartridge, and 300 mL of gaseous sample was collected. During gas sampling, N2 was introduced into the cartridge through the tip of the cartridge. After collecting the sample, the extraction needle was inserted into a heated gas chromatographic (GC) injection port, and the extracted PAHs were thermally desorbed followed by the GC separation on a fused-silica capillary column. The limits of quantification for Nap, Acy, Ace, and Flu were 36, 36, 15, and 36 ng through flame ionization detector and 3.6, 7.5, 7.5, and 36 ng through mass spectrometry, respectively.","PeriodicalId":10272,"journal":{"name":"Chromatography","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135513655","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}
ChromatographyPub Date : 2023-10-20DOI: 10.15583/jpchrom.2023.016
Kohei KAWABATA, Mai SANDANBATA, Hiroyuki NISHI
{"title":"Development of HPLC Optical Purity Testing Method of Denomapine and Application to Its Photostability","authors":"Kohei KAWABATA, Mai SANDANBATA, Hiroyuki NISHI","doi":"10.15583/jpchrom.2023.016","DOIUrl":"https://doi.org/10.15583/jpchrom.2023.016","url":null,"abstract":"Direct enantiomer separation of denopamine (DP, active form: R (-)-form), which is an optically active and an orally administrable cardiotonic agent, was investigated by HPLC with β-cyclodextrin (β-CD) immobilized chiral stationary phases (CSPs). Successful enantiomer separation under the reversed-phase mode was achieved by a β-CD having a phenyl moiety immobilized CSP with large resolution within 10 min. Optical purity testing and assay of tablets by the HPLC method developed were validated for specificity, linearity, and recovery. Validation results indicate the method is accurate and has a good linearity and sensitivity. Limit of detection and limit of quantitation of the minor enantiomer were 0.01% and 0.03%, respectively. Assay of DP tablets 5 mg by the internal standard method was also successfully achieved within 10 min. Further, photostability of DP was evaluated by this chiral HPLC method and the reversed-phase HPLC with an ODS column. Chemical structures of two photoproducts generated in an aqueous media were determined by LC-MS/MS, showing these were p-hydroxybenzaldehyde and 3,4-dimethoxyphenethylamine. Other than these two main photoproducts, low level (0.17%) of the minor enantiomer was detected.","PeriodicalId":10272,"journal":{"name":"Chromatography","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135513421","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}
{"title":"LVSEP Analysis of Cationic Analytes in Non-Aqueous Media on Cationic Polymer-Coated Channel Microchips","authors":"Fumihiko KITAGAWA, Yurie TAKAHASHI, Isoshi NUKATSUKA","doi":"10.15583/jpchrom.2023.019","DOIUrl":"https://doi.org/10.15583/jpchrom.2023.019","url":null,"abstract":"To improve the concentration sensitivity of cationic analytes in microchip electrophoresis, on-line sample preconcentration by a large-volume sample stacking with an electroosmotic flow pump (LVSEP) was performed using non-aqueous background solutions (BGSs) in cationic polymer-coated microchannels. In the LVSEP analyses using dimethyl sulfoxide-based BGS, however, poly(vinyl alcohol)/poly(allylamine) mixture-coated microchannel gave insufficient enrichments and broader peaks for cationic histamine. By employing a methanolic BGS containing (hydroxypropyl)methyl cellulose, on the other hand, good enrichments of histamine were achieved by LVSEP with the sensitive enhancement factor of 67. To our knowledge, this is first time that LVSEP analyses of cationic analytes were successfully realized in non-aqueous media.","PeriodicalId":10272,"journal":{"name":"Chromatography","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135513971","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}
{"title":"Enantioselective Analysis of Lactate, Hydroxybutyrates and Malate in Human Physiological Fluids Using a Three-Dimensional HPLC System","authors":"Hsin-Miao TSAI, Chin-Ling HSIEH, Chiharu ISHII, Takeyuki AKITA, Masashi MITA, Tomomi IDE, Jen-Ai LEE, Kenji HAMASE","doi":"10.15583/jpchrom.2023.015","DOIUrl":"https://doi.org/10.15583/jpchrom.2023.015","url":null,"abstract":"For the highly-selective analysis of lactic acid (LA), 2-hydroxybutyric acid (2HB), 3-hydroxybutyric acid (3HB) and malic acid (MA) enantiomers in human physiological fluids, a three-dimensional (3D) HPLC method following the fluorescence derivatization with 4-nitro-7-piperazino-2,1,3-benzoxadiazole has been designed and developed. The 3D-HPLC system was composed of reversed-phase, mixed-mode and enantioselective columns, and the conditions of all the dimensions were thoroughly investigated. In the first and second dimensions, the target hydroxy acids were separated from most of the interfering substances in the clinical samples. In the third dimension, the enantiomers were separated with resolution values higher than 3.47. The present method was validated by checking the calibration curves, precision and accuracy using standard solutions and human samples, and satisfactory results were acquired. Using the 3D-HPLC system, D-LA, L-LA, D-3HB, L-3HB and L-2HB were determined in the human plasma and urine (maleic acid enantiomers were not determined). The concentrations of the detected enantiomers in the human plasma were 6.2, 660, 34.0, 1.0 and 19.0 µM, and those in the human urine were 13.4, 88.3, 4.5, 3.7 and 4.5 µM, respectively.","PeriodicalId":10272,"journal":{"name":"Chromatography","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135514275","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}