Pub Date : 2020-06-20DOI: 10.15583/jpchrom.2020.008
I. Ueta, Masataka Sakamoto, K. Tani, Yoshihiro Saito
A gas chromatographic micro-packed column prepared with titanium dioxide (TiO 2 ) particles was developed. This study reports the fundamental retention behavior of the column for several organic and inorganic gaseous compounds, and quantitatively analyzes the high-temperature degradation behavior of the injected organic compounds. The anatase TiO 2 particles were prepared by hydrolysis of titanium (IV) isopropoxide. The particle size was classified as 150 – 180 μm. The micro-packed column was prepared by packing the classified TiO 2 particles into a stainless steel capillary of inner diameter of 1.0 mm and length of 1.0 m. The TiO 2 micro-packed column was connected to a conventional gas chromatograph equipped with a flame ionization detector or a thermal conductivity detector. The column showed high retentivity for carbon dioxide and also for organic compounds, achieving a baseline separation of methane and ethane. The TiO 2 packed column was highly thermally stable, with a temperature limit above 400°C. Above 300°C, the analytes injected into the column were thermally degraded by catalytic combustion of TiO 2 under N 2 carrier gas. On the other hand, the degradation was obtained above 200°C using air as the carrier gas.
{"title":"Titanium Dioxide as a Packing Material for Micro-Packed Column in Gas Chromatography","authors":"I. Ueta, Masataka Sakamoto, K. Tani, Yoshihiro Saito","doi":"10.15583/jpchrom.2020.008","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.008","url":null,"abstract":"A gas chromatographic micro-packed column prepared with titanium dioxide (TiO 2 ) particles was developed. This study reports the fundamental retention behavior of the column for several organic and inorganic gaseous compounds, and quantitatively analyzes the high-temperature degradation behavior of the injected organic compounds. The anatase TiO 2 particles were prepared by hydrolysis of titanium (IV) isopropoxide. The particle size was classified as 150 – 180 μm. The micro-packed column was prepared by packing the classified TiO 2 particles into a stainless steel capillary of inner diameter of 1.0 mm and length of 1.0 m. The TiO 2 micro-packed column was connected to a conventional gas chromatograph equipped with a flame ionization detector or a thermal conductivity detector. The column showed high retentivity for carbon dioxide and also for organic compounds, achieving a baseline separation of methane and ethane. The TiO 2 packed column was highly thermally stable, with a temperature limit above 400°C. Above 300°C, the analytes injected into the column were thermally degraded by catalytic combustion of TiO 2 under N 2 carrier gas. On the other hand, the degradation was obtained above 200°C using air as the carrier gas.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41451123","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 : 2020-06-20DOI: 10.15583/jpchrom.2020.005
Koichi Saito, Marika Eki, R. Ito
In order to explore the possibility of determining whether clenbuterol (CLB) was ingested unintentionally via meat products contaminated with CLB or taken intentionally for doping purposes by athletes, we conducted an in vitro study assuming in vivo chiral conversion of CLB. Enzymatic reaction using swine liver tissue or chemical reaction in artificial gastric juice was performed to clarify the chiral conversion of CLB enantiomers. LC/UV measurement revealed no chiral conversion in the enzymatic reaction and temperature-dependent chiral conversion in the artificial gastric juice where CLB finally racemized. From the calculated reaction rate, activation energy ( Ea ), and activation entropy ( ΔS ) in the chiral conversion reaction of R -CLB in artificial gastric juice, we expected that this chiral conversion would proceed slowly because E a was relatively high. After heating at 38°C for 2 h, only approximately 1% of CLB underwent chiral conversion. Therefore, when humans ingest meat products contaminated with CLB having a different enantiomeric ratio, chiral conversion hardly progresses in the stomach and such ingestion would have very little effect on the enantiomeric excess of CLB excreted in urine. This suggests that measuring urinary CLB enantiomeric ratio would reveal whether CLB was ingested unintentionally via CLB-contaminated meat products or taken intentionally.
{"title":"In vitro Study of Assumed in vivo Chiral Conversion of Clenbuterol","authors":"Koichi Saito, Marika Eki, R. Ito","doi":"10.15583/jpchrom.2020.005","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.005","url":null,"abstract":"In order to explore the possibility of determining whether clenbuterol (CLB) was ingested unintentionally via meat products contaminated with CLB or taken intentionally for doping purposes by athletes, we conducted an in vitro study assuming in vivo chiral conversion of CLB. Enzymatic reaction using swine liver tissue or chemical reaction in artificial gastric juice was performed to clarify the chiral conversion of CLB enantiomers. LC/UV measurement revealed no chiral conversion in the enzymatic reaction and temperature-dependent chiral conversion in the artificial gastric juice where CLB finally racemized. From the calculated reaction rate, activation energy ( Ea ), and activation entropy ( ΔS ) in the chiral conversion reaction of R -CLB in artificial gastric juice, we expected that this chiral conversion would proceed slowly because E a was relatively high. After heating at 38°C for 2 h, only approximately 1% of CLB underwent chiral conversion. Therefore, when humans ingest meat products contaminated with CLB having a different enantiomeric ratio, chiral conversion hardly progresses in the stomach and such ingestion would have very little effect on the enantiomeric excess of CLB excreted in urine. This suggests that measuring urinary CLB enantiomeric ratio would reveal whether CLB was ingested unintentionally via CLB-contaminated meat products or taken intentionally.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46101233","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 : 2020-06-20DOI: 10.15583/jpchrom.2020.006
Kazumasa Zaima, R. Koga, Riku Motegi, Hanae Sato, S. Kitanaka, Y. Ito, K. Shinomiya
Separation of flavanonol, phenylcoumaran and flavonolignans in Silybum marianum was examined using high-speed countercurrent chromatography (HSCCC). In order to prepare analytical standards, a flavanonol of aromadendrin (87.4% purity, 7.8 mg), three phenylcoumarans of jatrointelignan D (84.5% purity, 13.2 mg), dehydrodiconiferyl alcohol (76.1% purity, 1.4 mg) and dihydrodehydrodiconiferyl alcohol (93.0% purity, 5.8 mg), and three flavonolignans of silybin (88.8% purity, 35.6 mg), silydianin (99.3% purity, 25.1 mg) and silychristin (96.9% purity, 12.6 mg) were separated from the seeds of S. marianum using common column chromatography and ODS-HPLC, and identified by 1H and 13C NMR spectra. Then, HSCCC with the hexane/ethyl acetate/methanol/water (3 : 7 : 4 : 6, v/v) system was applied to the separation of aromadendrin, jatrointelignan D, silydianin and silybin. In this separation, it was revealed that silybin and silydianin were successfully separated from each other. The present HSCCC system was directly applied to the ethyl acetate extract and resulted in the separation of silybin. The overall results suggested that HSCCC is useful for the separation of bioactive compounds in S. marianum.
{"title":"Application of High-Speed Countercurrent Chromatography to the Separation of Flavanonol, Phenylcoumaran and Flavonolignans in Silybum marianum","authors":"Kazumasa Zaima, R. Koga, Riku Motegi, Hanae Sato, S. Kitanaka, Y. Ito, K. Shinomiya","doi":"10.15583/jpchrom.2020.006","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.006","url":null,"abstract":"Separation of flavanonol, phenylcoumaran and flavonolignans in Silybum marianum was examined using high-speed countercurrent chromatography (HSCCC). In order to prepare analytical standards, a flavanonol of aromadendrin (87.4% purity, 7.8 mg), three phenylcoumarans of jatrointelignan D (84.5% purity, 13.2 mg), dehydrodiconiferyl alcohol (76.1% purity, 1.4 mg) and dihydrodehydrodiconiferyl alcohol (93.0% purity, 5.8 mg), and three flavonolignans of silybin (88.8% purity, 35.6 mg), silydianin (99.3% purity, 25.1 mg) and silychristin (96.9% purity, 12.6 mg) were separated from the seeds of S. marianum using common column chromatography and ODS-HPLC, and identified by 1H and 13C NMR spectra. Then, HSCCC with the hexane/ethyl acetate/methanol/water (3 : 7 : 4 : 6, v/v) system was applied to the separation of aromadendrin, jatrointelignan D, silydianin and silybin. In this separation, it was revealed that silybin and silydianin were successfully separated from each other. The present HSCCC system was directly applied to the ethyl acetate extract and resulted in the separation of silybin. The overall results suggested that HSCCC is useful for the separation of bioactive compounds in S. marianum.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67104144","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 : 2020-02-22DOI: 10.15583/jpchrom.2020.002
I. Ueta, Naho Sekiguchi, A. Suzuki, Yuta Kobayashi, T. Kuwabara, Yoshihiro Saito
An extraction capillary packed with a polyethylene terephthalate nanofiber-sheet was applied for the extraction of five water soluble polycyclic aromatic hydrocarbons (PAHs, including naphthalene (Nap), fluorene (Flu), phenanthrene (Phe), fluoranthene (Flt), and pyrene (Pyr)), in water samples. The extracted PAHs were eluted with acetonitrile, and on-line injected into a high-performance liquid chromatographic system coupled with a fluorescence detector. The limit of detections of the method for Nap, Flu, Phe, Flt, and Pyr were 1.0, 1.0, 0.2, 0.5, and 0.2 ng/mL, respectively, at a sample loading volume of 1.0 mL. The spiked recoveries of the analyte PAHs were in the range of 97.3 to 102% upon spiking the PAHs into tap water and river water samples.
{"title":"Carbon Dioxide Laser Supersonic Drawing Nanofiber Sheet for Extraction of Polycyclic Aromatic Hydrocarbons in Water Samples","authors":"I. Ueta, Naho Sekiguchi, A. Suzuki, Yuta Kobayashi, T. Kuwabara, Yoshihiro Saito","doi":"10.15583/jpchrom.2020.002","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.002","url":null,"abstract":"An extraction capillary packed with a polyethylene terephthalate nanofiber-sheet was applied for the extraction of five water soluble polycyclic aromatic hydrocarbons (PAHs, including naphthalene (Nap), fluorene (Flu), phenanthrene (Phe), fluoranthene (Flt), and pyrene (Pyr)), in water samples. The extracted PAHs were eluted with acetonitrile, and on-line injected into a high-performance liquid chromatographic system coupled with a fluorescence detector. The limit of detections of the method for Nap, Flu, Phe, Flt, and Pyr were 1.0, 1.0, 0.2, 0.5, and 0.2 ng/mL, respectively, at a sample loading volume of 1.0 mL. The spiked recoveries of the analyte PAHs were in the range of 97.3 to 102% upon spiking the PAHs into tap water and river water samples.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45830627","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 : 2020-02-20DOI: 10.15583/jpchrom.2019.026
Kohei Kawabata, Shiori Akimoto, H. Nishi
To determine the fate and behavior of pharmaceuticals in the aquatic environment, in this study, we investigated the photo-conversion of phenytoin (PH), which is one of the antepilepsy drug, induced by ultraviolet light (UV) irradiation in the aqueous media. The degradation of PH and the generation of its photoproducts were monitored by means of high-performance liquid chromatography (HPLC). Based on the fragmentation patterns in electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS/MS) and coupling patterns in nuclear magnetic resonance (NMR) spectrum, the main photoproduct of PH was determined as benzophenone. Evaluation of toxicity by means of luminescent bacteria test (ISO11348) indicated that a PH solution was nontoxic, whereas a UV-irradiated PH solution and a benzophenone solution were toxic (EC 50 : 19.46 mg/L and 24.40 mg/L). It was shown that benzophenone has a contribution to the increase of ecotoxicity of PH solution for luminescent bacteria after UV irradiation. This is the first report of the photo-conversion of PH to benzophenone induced by UV irradiation in the absence of photo-catalysts. These results indicate that the importance of evaluating not only parent compounds but also its photoproducts for the risk assessment of pharmaceuticals in the aquatic environment.
{"title":"Photo-Conversion of Phenytoin to Ecotoxicological Substance Benzophenone by Ultraviolet Light Irradiation in Aqueous Media","authors":"Kohei Kawabata, Shiori Akimoto, H. Nishi","doi":"10.15583/jpchrom.2019.026","DOIUrl":"https://doi.org/10.15583/jpchrom.2019.026","url":null,"abstract":"To determine the fate and behavior of pharmaceuticals in the aquatic environment, in this study, we investigated the photo-conversion of phenytoin (PH), which is one of the antepilepsy drug, induced by ultraviolet light (UV) irradiation in the aqueous media. The degradation of PH and the generation of its photoproducts were monitored by means of high-performance liquid chromatography (HPLC). Based on the fragmentation patterns in electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS/MS) and coupling patterns in nuclear magnetic resonance (NMR) spectrum, the main photoproduct of PH was determined as benzophenone. Evaluation of toxicity by means of luminescent bacteria test (ISO11348) indicated that a PH solution was nontoxic, whereas a UV-irradiated PH solution and a benzophenone solution were toxic (EC 50 : 19.46 mg/L and 24.40 mg/L). It was shown that benzophenone has a contribution to the increase of ecotoxicity of PH solution for luminescent bacteria after UV irradiation. This is the first report of the photo-conversion of PH to benzophenone induced by UV irradiation in the absence of photo-catalysts. These results indicate that the importance of evaluating not only parent compounds but also its photoproducts for the risk assessment of pharmaceuticals in the aquatic environment.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44208389","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 : 2020-02-20DOI: 10.15583/jpchrom.2020.004
Chiharu Ishii, Aogu Furusho, C. Hsieh, K. Hamase
Chiral amino acid analysis, especially the determination of trace levels of D-enantiomers, is currently gathering attention in a variety of research areas including the food/clinical sciences. These D-amino acids had long been believed to be absent in the higher animals. However, by the advances of analytical technologies, some of the D-enantiomers are found in mammals including humans and increasingly recognized as novel physiologically-active substances and/or biomarkers. For the determination of these D-amino acids and related compounds in real world samples, utilization of sensitive and selective methods is essential and multi-dimensional HPLC is one of the straightforward approaches. In the present review, two/three-dimensional HPLC methods and biological/medical applications focusing on our current studies are summarized.
{"title":"Multi-Dimensional High-Performance Liquid Chromatographic Determination of Chiral Amino Acids and Related Compounds in Real World Samples","authors":"Chiharu Ishii, Aogu Furusho, C. Hsieh, K. Hamase","doi":"10.15583/jpchrom.2020.004","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.004","url":null,"abstract":"Chiral amino acid analysis, especially the determination of trace levels of D-enantiomers, is currently gathering attention in a variety of research areas including the food/clinical sciences. These D-amino acids had long been believed to be absent in the higher animals. However, by the advances of analytical technologies, some of the D-enantiomers are found in mammals including humans and increasingly recognized as novel physiologically-active substances and/or biomarkers. For the determination of these D-amino acids and related compounds in real world samples, utilization of sensitive and selective methods is essential and multi-dimensional HPLC is one of the straightforward approaches. In the present review, two/three-dimensional HPLC methods and biological/medical applications focusing on our current studies are summarized.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/jpchrom.2020.004","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43873688","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 : 2020-02-20DOI: 10.15583/jpchrom.2020.001
Masamitsu Maekawa, N. Mano
Niemann–Pick disease type C (NPC) is an autosomal recessive disorder that features progressive neurodegeneration. Because NPC patients have mutations in NPC1 or NPC2 cholesterol transporting proteins, failures in cholesterol and other lipid trafficking occur. NPC patients represent a wide clinical spectrum in terms of age of onset and type of symptoms. Because conventional diagnostic methods are time-consuming and complicated, biomarker tests have attracted increased attention. In this review, recently reported biomarkers for NPC are discussed in detail. For example, oxysterols and some cholenoic acid conjugates, metabolized from excess cholesterol in NPC cells, can be detected in urine or plasma. In addition, two types of lysosphingolipids, sphingosylphosphorylcholine and glycosylsphingosine, are present at increased concentrations in NPC patients. A more recently discovered biomarker is N-palmitoyl-O-phosphorylcholine, previously called “lysosphingomyelin-509.” These biomarkers are helpful for the early diagnosis of NPC and may contribute to a good prognosis for NPC patients.
尼曼-皮克病C型(NPC)是一种常染色体隐性遗传病，以进行性神经变性为特征。由于鼻咽癌患者的NPC1或NPC2胆固醇转运蛋白发生突变，导致胆固醇和其他脂质转运失败。鼻咽癌患者在发病年龄和症状类型方面表现出广泛的临床谱。由于传统的诊断方法耗时且复杂，生物标志物测试引起了越来越多的关注。本文就近年来报道的鼻咽癌生物标志物作一综述。例如，在尿液或血浆中可检测到由鼻咽癌细胞中过量胆固醇代谢而成的氧化甾醇和某些胆烯酸缀合物。此外，两种类型的溶鞘脂，鞘鞘sylphospylcholine和鞘鞘糖苷，在鼻咽癌患者中浓度升高。最近发现的一种生物标志物是n-棕榈酰- o -磷胆碱，以前被称为“溶磷脂-509”。这些生物标志物有助于鼻咽癌的早期诊断，并可能有助于鼻咽癌患者的良好预后。
{"title":"Identification and Evaluation of Biomarkers for Niemann-Pick Disease Type C Based on Chemical Analysis Techniques","authors":"Masamitsu Maekawa, N. Mano","doi":"10.15583/jpchrom.2020.001","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.001","url":null,"abstract":"Niemann–Pick disease type C (NPC) is an autosomal recessive disorder that features progressive neurodegeneration. Because NPC patients have mutations in NPC1 or NPC2 cholesterol transporting proteins, failures in cholesterol and other lipid trafficking occur. NPC patients represent a wide clinical spectrum in terms of age of onset and type of symptoms. Because conventional diagnostic methods are time-consuming and complicated, biomarker tests have attracted increased attention. In this review, recently reported biomarkers for NPC are discussed in detail. For example, oxysterols and some cholenoic acid conjugates, metabolized from excess cholesterol in NPC cells, can be detected in urine or plasma. In addition, two types of lysosphingolipids, sphingosylphosphorylcholine and glycosylsphingosine, are present at increased concentrations in NPC patients. A more recently discovered biomarker is N-palmitoyl-O-phosphorylcholine, previously called “lysosphingomyelin-509.” These biomarkers are helpful for the early diagnosis of NPC and may contribute to a good prognosis for NPC patients.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"41 1","pages":"19-29"},"PeriodicalIF":0.0,"publicationDate":"2020-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43913571","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 : 2020-02-20DOI: 10.15583/jpchrom.2020.003
T. Naito
Microfluidic device is capable of reducing amount of sample consumption, shortening the analysis time, and miniaturizing instruments. Many applications of microfluidic devices have been developed not only in chemical analysis but also in medical diagnosis, and the food and agricultural industries. Electrophoresis or chromatography in a microfluidic device has improved the speed, reproducibility and separation resolution. Some of them have been integrated with complex experimental functionality on a small substrate, of which concept is known as micro total analysis systems. To build up a system, microfluidic components that carry out an experimental functionality in a microfluidic channel and novel technology to support the developments of microfluidic components are indispensable. In this review, three-dimensional (3D) fabrication by thiol-ene quick reaction, sample injection with an inkjet ejector, and molecular detection based on electroosmosis are focused biefly. The 3D fabrication realizes to make various 3D microstructures that conventional fabrication method cannot make without specific equipment. The sample injection by using inkjet technology can apply tiny amount of sample solution into multiple microfluidic channel on some precise spots, which leads to rapid analysis with high accuracy. The electroosmosis-based molecular detection indicates a possibility to develop a new portable device without any peripherals for detection or pretreatment for specimen labeling.
{"title":"Development of Microfluidic Components for Micro Total Analysis Systems","authors":"T. Naito","doi":"10.15583/jpchrom.2020.003","DOIUrl":"https://doi.org/10.15583/jpchrom.2020.003","url":null,"abstract":"Microfluidic device is capable of reducing amount of sample consumption, shortening the analysis time, and miniaturizing instruments. Many applications of microfluidic devices have been developed not only in chemical analysis but also in medical diagnosis, and the food and agricultural industries. Electrophoresis or chromatography in a microfluidic device has improved the speed, reproducibility and separation resolution. Some of them have been integrated with complex experimental functionality on a small substrate, of which concept is known as micro total analysis systems. To build up a system, microfluidic components that carry out an experimental functionality in a microfluidic channel and novel technology to support the developments of microfluidic components are indispensable. In this review, three-dimensional (3D) fabrication by thiol-ene quick reaction, sample injection with an inkjet ejector, and molecular detection based on electroosmosis are focused biefly. The 3D fabrication realizes to make various 3D microstructures that conventional fabrication method cannot make without specific equipment. The sample injection by using inkjet technology can apply tiny amount of sample solution into multiple microfluidic channel on some precise spots, which leads to rapid analysis with high accuracy. The electroosmosis-based molecular detection indicates a possibility to develop a new portable device without any peripherals for detection or pretreatment for specimen labeling.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":"41 1","pages":"31-37"},"PeriodicalIF":0.0,"publicationDate":"2020-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.15583/jpchrom.2020.003","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46264769","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 : 2020-02-20DOI: 10.15583/jpchrom.2019.027
Y. Esaka, Eriko Tokoro, Saki Kunishima, Takuhei Yamamoto, Hiroyuki Kojima, Takahashi Tatsuji, Hiroya Murakami, B. Uno
Quantification of four extracellular matrices commonly found in foods with functional claims was conducted using capillary zone electrophoresis with direct ultraviolet (UV) absorbance detection at 200 nm. The four polymeric compounds, namely, proteoglycan, chondroitin sulfate, hyaluronic acid, and collagen, were separated with 100 mM borate buffer (pH 10.0) using capillaries coated with poly-N,N-dimethylacrylamide on the inner wall, which almost completely suppressed the electroosmotic flow to give reproducible migration times for the analytes. The addition of 5 mM sodium dodecyl sulfate to the running solutions improved the shapes of the peaks and the linearity of the calibration curves. Some commercial products, including the extracellular matrices under investigation, were analyzed with the method developed.
采用毛细管区带电泳直接紫外(UV)检测，在200 nm下对功能性食品中常见的4种细胞外基质进行了定量分析。蛋白多糖、硫酸软骨素、透明质酸和胶原蛋白这四种高分子化合物，用100 mM硼酸盐缓冲液(pH 10.0)分离，内壁涂有聚n, n -二甲基丙烯酰胺的毛细管，几乎完全抑制了电渗透流动，为分析物提供了可重复的迁移时间。在运行液中加入5mm十二烷基硫酸钠改善了峰的形状和校准曲线的线性度。一些商业产品，包括正在研究的细胞外基质，用该方法进行了分析。
{"title":"Development of a Capillary Zone Electrophoresis Method for the Analysis of Four Extracellular Matrices Commonly Found in Foods with Functional Claims","authors":"Y. Esaka, Eriko Tokoro, Saki Kunishima, Takuhei Yamamoto, Hiroyuki Kojima, Takahashi Tatsuji, Hiroya Murakami, B. Uno","doi":"10.15583/jpchrom.2019.027","DOIUrl":"https://doi.org/10.15583/jpchrom.2019.027","url":null,"abstract":"Quantification of four extracellular matrices commonly found in foods with functional claims was conducted using capillary zone electrophoresis with direct ultraviolet (UV) absorbance detection at 200 nm. The four polymeric compounds, namely, proteoglycan, chondroitin sulfate, hyaluronic acid, and collagen, were separated with 100 mM borate buffer (pH 10.0) using capillaries coated with poly-N,N-dimethylacrylamide on the inner wall, which almost completely suppressed the electroosmotic flow to give reproducible migration times for the analytes. The addition of 5 mM sodium dodecyl sulfate to the running solutions improved the shapes of the peaks and the linearity of the calibration curves. Some commercial products, including the extracellular matrices under investigation, were analyzed with the method developed.","PeriodicalId":91226,"journal":{"name":"Chromatography (Basel)","volume":" ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43294619","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 : 2020-02-20DOI: 10.15583/jpchrom.2019.024
Yoshiyuki Kobayashi, Masakadzu Yato, R. Ito, Koichi Saito
An enantioselective analytical method for the determination of synephrine, an ingredient in health food, by liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) was developed. By derivatizing synephrine with FMOC and using TCI Chiral MB-S as the chiral column, FMOC-synephrine enantiomers were well separated. The electrospray ionization (ESI) negative mode was adopted for TOF-MS measurement. Good linearity ( r > 0.999) was obtained in the concentration range of 0.5 to 50 μg/mL. The limit of detection (LOD, S / N = 3) and the limit of quantification (LOQ, S / N > 10) were 0.25 μg/mL and 0.5 μg/mL, respectively. The intra-day and inter-day accuracy of synephrine enantiomers at the LOQ level (0.5 μg/mL), the intermediate concentration level (10 μg/mL), and the high concentration level (50 μg/mL) ranged from 90.0 to 107.4%. The intra-day and inter-day precisions were ≤ 9.24% and ≤ 10.63%, respectively. As a result of analyzing synephrine-containing health foods using this method, approximately half of the products showed high optical purity with 80–100% enantiomeric excess of the l -isomer. In contrast, nearly 20% of the products contained racemate with 0–50% enantiomeric excess, and variations in optical purity were observed for the products. It was speculated that the l -isomer could be converted into the d -isomer during the manufacturing process.
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