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Counter-Current Chromatographic Separation of Nucleic Acid Constituents with a Polar Volatile Organic-Aqueous Two-Phase Solvent Systems with ELSD Detection. 极性挥发性有机-水两相溶剂体系逆流色谱分离核酸成分的ELSD检测。
The open analytical chemistry journal Pub Date : 2012-01-01 DOI: 10.2174/1874065001206010009
Yoichi Shibusawa, Go Morikawa, Akio Yanagida, Yoichiro Ito
{"title":"Counter-Current Chromatographic Separation of Nucleic Acid Constituents with a Polar Volatile Organic-Aqueous Two-Phase Solvent Systems with ELSD Detection.","authors":"Yoichi Shibusawa,&nbsp;Go Morikawa,&nbsp;Akio Yanagida,&nbsp;Yoichiro Ito","doi":"10.2174/1874065001206010009","DOIUrl":"https://doi.org/10.2174/1874065001206010009","url":null,"abstract":"<p><p>Highly hydrophilic volatile organic/aqueous two-phase solvent systems containing an organic salt such as, acetonitrile/800 mM and 1200 mM ammonium acetate (1 : 1, v/v) were efficiently utilized for high-speed counter-current chromatography (HSCCC) to separate hydrophilic compounds. The retention of the upper and the lower stationary phases in the column of the cross-axis coil planet centrifuge (CCC instrument) was studied by changing the flow-rate of the mobile phase (1.0-3.0 ml/min). Using the acetonitrile/800 mM ammonium acetate two-phase solvent system, the stationary phase was retained at 46.3% relative to the total column capacity of 65 ml by the reversed-phase elution mode at a flow-rate of 1.0 ml/min. The best retention of the stationary upper phase of 51.5% was obtained by the solvent system of the acetonitrile/1200 mM ammonium acetate at the above flow-rate. With the acetonitrile/800 mM ammonium acetate system the base line separation of adenine and adenosine monophosphate (AMP) detected by evaporative light scattering detector (ELSD) and UV was achieved with lower phase mobile at a flow-rate of 1.0 ml/min within 70 min.</p>","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"6 ","pages":"9-14"},"PeriodicalIF":0.0,"publicationDate":"2012-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://ftp.ncbi.nlm.nih.gov/pub/pmc/oa_pdf/2c/ab/nihms563430.PMC3952559.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"32180438","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mass Spectral Fragmentation Studies of Coumarin-Type Compounds Using GC High-Resolution MS 香豆素类化合物的质谱碎片化研究
The open analytical chemistry journal Pub Date : 2011-11-30 DOI: 10.2174/187406500115010027
V. Lopez-Avila, G. Yefchak
{"title":"Mass Spectral Fragmentation Studies of Coumarin-Type Compounds Using GC High-Resolution MS","authors":"V. Lopez-Avila, G. Yefchak","doi":"10.2174/187406500115010027","DOIUrl":"https://doi.org/10.2174/187406500115010027","url":null,"abstract":"The present study was undertaken to investigate fragmentation of a set of thirteen coumarins that bear amino-, alkylamino-, alkyl-, fluoroalkyl-groups, and heterocyclic rings, in a high-resolution (>10,000) quadrupole time-of-flight mass spectrometer equipped with an the electron ionization source and interfaced to a gas chromatograph. We have demonstrated how our data processing software is used to generate molecular formulas from high-resolution accurate mass measurements and isotope ratios, and have shown that only with a high-resolution MS can one distinguish between the loss of CO, C2H4, or CH2N. EI mass spectra are shown for all coumarins tested here, and proposed fragmentation pathways based on the high-resolution MS data are proposed for two coumarins.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"51 1","pages":"27-36"},"PeriodicalIF":0.0,"publicationDate":"2011-11-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79536543","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: 6
Determination of Putrescine and Tyramine in Fish by Micellar Liquid Chromatography with UV Detection Using Direct Injection 直接进样胶束液相色谱-紫外检测法测定鱼中的腐胺和酪胺
The open analytical chemistry journal Pub Date : 2011-02-18 DOI: 10.2174/187406500115010022
Mei-Liang Chin-Chen, D. Bose, J. Esteve-Romero, J. Peris-Vicente, M. Rambla-Alegre, S. Carda‐Broch
{"title":"Determination of Putrescine and Tyramine in Fish by Micellar Liquid Chromatography with UV Detection Using Direct Injection","authors":"Mei-Liang Chin-Chen, D. Bose, J. Esteve-Romero, J. Peris-Vicente, M. Rambla-Alegre, S. Carda‐Broch","doi":"10.2174/187406500115010022","DOIUrl":"https://doi.org/10.2174/187406500115010022","url":null,"abstract":"This paper shows how fish samples could be directly injected into a chromatograph, without any previous extraction, using micellar liquid chromatography, taking as an example the determination of two biogenic amines: putrescine and tyramine, derivatized with 3,5-dinitrobenzoyl chloride. First, the method has been optimized, using an interpretive model, and the best conditions for analysis were: mobile phase containing 0.15 M SDS-6% (v/v) butanol-pH 7, C18 column (125 � 0.46 mm, 5 μm particle size), UV detection of derivatives set at 260 nm. Second, the method has been validated using spiked samples following the guidelines proposed by the US Food and Drug Administration: linear in the range from 0.5 to 1000 ppm (r 2 >0.999), detection limits of 30 and 40 ppb for putrescine and tyramine, respectively, a 500 ppb limit of quantification in both cases, intra- and inter-day precision (RSD) below 2%, and accuracy between 99.5% and 102.7%. The method is adequate for routine analysis in the determination of these compounds in fish sauces.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"17 1","pages":"22-26"},"PeriodicalIF":0.0,"publicationDate":"2011-02-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85822355","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: 22
The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques 方法验证在电分析药物分析中的作用和地位
The open analytical chemistry journal Pub Date : 2011-01-25 DOI: 10.2174/1874065001005010001
M. Gumustas, S. Ozkan
{"title":"The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques","authors":"M. Gumustas, S. Ozkan","doi":"10.2174/1874065001005010001","DOIUrl":"https://doi.org/10.2174/1874065001005010001","url":null,"abstract":"Electroanalytical methods are chosen for the sensitive analysis of pharmaceutically active compounds in their dosage forms and biological samples. Electroanalytical method validation is the process used to confirm that the determination procedure employed for a specific test is suitable for its intended use like other analytical methods. Results from electroanalytical method validation can be used to judge the quality, applicability, accuracy, reliability and","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"21 1","pages":"1-21"},"PeriodicalIF":0.0,"publicationDate":"2011-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76579400","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: 91
Comparison of Purification Efficiencies of Different Affinity Separation Techniques 不同亲和分离技术纯化效率的比较
The open analytical chemistry journal Pub Date : 2010-07-16 DOI: 10.2174/1874065001004010027
M. Kötke, H. Rosenfeld, S. Peper, B. Niemeyer
{"title":"Comparison of Purification Efficiencies of Different Affinity Separation Techniques","authors":"M. Kötke, H. Rosenfeld, S. Peper, B. Niemeyer","doi":"10.2174/1874065001004010027","DOIUrl":"https://doi.org/10.2174/1874065001004010027","url":null,"abstract":"An affinity separation method for the isolation of recombinantly produced benzoylformiate decarboxylase (BFD) is presented based on the interaction of the enzyme to its cofactor. Enzyme/cofactor interactions are well suited for affinity purification processes with regard to its high affinity and selectivity. Problems can be induced due to harsh desorption conditions that probably diminish the activity of the purified enzyme. The implementation of boronic acids to immobilize the cofactor introduces a gentle release by a simple pH shift from 8.5 to 6. The disadvantages of m- aminophenyl boronic acids are the high nonspecific adsorption induced by the introduction of a positive charge and a hydrophobic phenyl ring. It was shown that the disadvantages prevail and boronic acid resins are not suitable for protein purification from complex matrices. In contrast to the affinity separation method, where the cofactor was directly immobilized onto the support, a better separation performance could be achieved, which is reflected by a purification factor of 4.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"71 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2010-07-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85375149","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: 0
Metals Determination in Biodiesel (B100) by ICP-OES with Microwave Assisted Acid Digestion 微波辅助酸消化ICP-OES法测定生物柴油(B100)中的金属
The open analytical chemistry journal Pub Date : 2010-04-22 DOI: 10.2174/1874065001004010018
J. Iqbal, William A. Carney, Shelly LaCaze, C. Theegala
{"title":"Metals Determination in Biodiesel (B100) by ICP-OES with Microwave Assisted Acid Digestion","authors":"J. Iqbal, William A. Carney, Shelly LaCaze, C. Theegala","doi":"10.2174/1874065001004010018","DOIUrl":"https://doi.org/10.2174/1874065001004010018","url":null,"abstract":"Elemental composition of biodiesel is required for product quality-control, auto-engine life, emissions control, and researching appropriate additives. The use of microwave assisted acid digestion reaction system to prepare neat biodiesel (B100) samples in an aqueous medium for simultaneous inductively coupled plasma optical emission spectrometer (ICP-OES) analyses is reported. Biodiesel produced by transesterification reaction was subjected to the test method using calibration standards prepared in an aqueous medium. Significant correlation for the spiked B100 samples, instrument detection limits, accuracy, and precision data showed that elemental concentrations can easily be determined within the specified limits. The method avoids switching any of the ICP-OES accessories required for high organic loads. This method is most appropriately devised for biodiesel analysis than petrochemicals analysis. A consistent quality assurance program is necessary to avoid performance issues in vehicle engines and to ensure sustainable growth of biodiesel production. Inorganic constituents in the final product can promote residue build up in the engine, cause corrosion and ultimately affect engine life. Elements introduced during production process (Na, K, Ca, and Mg) are of particular concern, while other elements present in the feedstock (P, S, and Zn), or used as additives (Si, Mn, Cr, Fe, and Ni) require monitoring in order to avoid undesirable combustion products in the engines (6). Since metallic elements in fuel are undesirable even at lower concentrations, their determination in fuel is necessary to evaluate fuel quality, to see their effect on auto engines, and to control environmental pollution.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2010-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89593129","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: 40
A Rapid HPLC Analysis for Dermal Penetration: The Case Study of 4-Chloro-3-Methylphenol (CMP) from Metal Working Fluid Trim VX 金属加工液Trim VX中4-氯-3-甲基苯酚(CMP)的快速高效液相色谱分析
The open analytical chemistry journal Pub Date : 2010-04-02 DOI: 10.2174/1874065001004010010
L. Zang, A. Barbero, H. Frasch
{"title":"A Rapid HPLC Analysis for Dermal Penetration: The Case Study of 4-Chloro-3-Methylphenol (CMP) from Metal Working Fluid Trim VX","authors":"L. Zang, A. Barbero, H. Frasch","doi":"10.2174/1874065001004010010","DOIUrl":"https://doi.org/10.2174/1874065001004010010","url":null,"abstract":"A rapid and simple HPLC method has been developed for the determination of 4-chloro-3-methylphenol (CMP) in the metal working fluid (MWF), Trim VX and in experiments designed to measure the dermal penetration of CMP from MWF. The method used 2-methyl-4,6-dinitrophenol as an internal standard (IS). Water was used as the extraction solvent. The retention times of CMP and internal standard (IS) were 5.56 and 6.67 min, respectively. The standard plots of CMP are linear over the range of 62.5 2,500 ng·mL -1 with correlation coefficients of 0.999. The limit of quantification (LOQ) for CMP was estimated to be 62.5 ng·mL -1 and the limit of detection (LOD) was approached to be 20 ng·mL -1 . Reproducibility of the sample handling and HPLC analysis had a relative standard deviation (RSD) of less than 6%. The average recoveries for the analyte in Trim VX were better than 92%. Using the method, we found that Trim VX contains 2% CMP. In our preliminary dermal penetration study, the permeability coefficient kp and lag time were estimated to be 4.88 10 -3 cm·h -1 and 1.65 h, respectively.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2010-04-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90203698","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: 6
A Plasma Metabolomic Investigation of Colorectal Cancer Patients by Liquid Chromatography-Mass Spectrometry 用液相色谱-质谱法研究结直肠癌患者血浆代谢组学
The open analytical chemistry journal Pub Date : 2010-01-15 DOI: 10.2174/1874065001004010001
Y. Fukui, K. Itoh
{"title":"A Plasma Metabolomic Investigation of Colorectal Cancer Patients by Liquid Chromatography-Mass Spectrometry","authors":"Y. Fukui, K. Itoh","doi":"10.2174/1874065001004010001","DOIUrl":"https://doi.org/10.2174/1874065001004010001","url":null,"abstract":"Due to hypoxic conditions, colorectal cancer (CRC) tissues have a specific metabolism compared with normal mucosa, and this study aimed to investigate blood plasma metabolite differences between CRC patients and healthy subjects. Non-targeted methods have previously been used to characterize CRC disease diagnosis and identify small molecules in biological samples, but here we used a metabolomic approach based on liquid chromatography-mass spectrometry (LC-MS) of blood plasma from CRC patients (n=10) and healthy subjects (n=10). The analysis detected 130 identified compounds including free amino acids, fatty acids and nucleotides. Of these, many free amino acids were decreased in CRC patients while nucleotide-related and stress-related metabolites were increased in CRC patients compared with healthy subjects. Multivariate analysis clearly separated CRC patients and healthy subjects. These results demonstrate that plasma metabolite would reflects tumoral specific metabolism and metabolomic profiling of blood plasma using LC-MS is a valuable tool for characterizing CRC patients based on plasma metabolite diagnostic markers.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"72 1","pages":"1-9"},"PeriodicalIF":0.0,"publicationDate":"2010-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91358650","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
Identification of Compounds in Commercial Kava Extracts by Gas Chromatography with Electron Ionization High-Resolution Mass Spectrometry 用气相色谱-电子电离高分辨率质谱法鉴定商业卡瓦提取物中的化合物
The open analytical chemistry journal Pub Date : 2009-10-21 DOI: 10.2174/1874065000903010022
V. Lopez-Avila, G. Yefchak
{"title":"Identification of Compounds in Commercial Kava Extracts by Gas Chromatography with Electron Ionization High-Resolution Mass Spectrometry","authors":"V. Lopez-Avila, G. Yefchak","doi":"10.2174/1874065000903010022","DOIUrl":"https://doi.org/10.2174/1874065000903010022","url":null,"abstract":"This paper discusses the identification of kava lactones and related compounds by gas chromatography (GC) and quadrupole time-of-flight mass spectrometry (QTOFMS) with an electron ionization source. Three herbal preparations from different sources were analyzed by both GC-low-resolution MS and GC-high-resolution MS. The exact mass measurements generated with a research QTOFMS with mass accuracies in the low ppm range were combined with the isotope abundance ratios to confirm the presence of kava lactones and to identify additional compounds present in the Kava extracts. Although the availability of standards is of upmost importance to unequivocally confirm compound identities, the combination of accurate mass ( 10,000) and literature information on the approximate composition of the herbal extracts provides a powerful analytical tool to help identify organic compounds in herbal extracts.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"135 1","pages":"22-31"},"PeriodicalIF":0.0,"publicationDate":"2009-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86293511","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: 5
Binding of Low-Molecular-Weight Cationic Ligands to Chondroitin Sulfate as Studied by Capillary Electrophoresis Frontal Analysis 毛细管电泳正面分析研究低分子量阳离子配体与硫酸软骨素的结合
The open analytical chemistry journal Pub Date : 2009-09-25 DOI: 10.2174/1874065000903010016
Jesper Østergaard, Henrik Jensen, S. Larsen, C. Larsen
{"title":"Binding of Low-Molecular-Weight Cationic Ligands to Chondroitin Sulfate as Studied by Capillary Electrophoresis Frontal Analysis","authors":"Jesper Østergaard, Henrik Jensen, S. Larsen, C. Larsen","doi":"10.2174/1874065000903010016","DOIUrl":"https://doi.org/10.2174/1874065000903010016","url":null,"abstract":"The feasibility of capillary electrophoresis frontal analysis for the study of low-molecular-weight ligand- chondroitin sulfate interactions was investigated. The interaction of the 7 cationic ligands (lidocaine, propranolol, scopolamine, N-methyl scopolamine, N-butyl scopolamine, 2-propylisochinolinium, and methyl viologen) with the glycosaminoglycan chondroitin sulfate was investigated in 0.067 M phosphate buffer, pH 7.4, at 25 o C. A frontal analysis method with a short analysis time, suitable for ranking ligands according to degree of complexation for chondroitin sulfate was developed. The double charged ligand methyl viologen possessed the highest affinity for chondroitin sulfate. Linear binding isotherms were obtained and apparent association constants were determined. Capillary electrophoresis frontal analysis may be an attractive tool for characterization of ligand-glycosaminoglycan interactions.","PeriodicalId":90363,"journal":{"name":"The open analytical chemistry journal","volume":"476 1","pages":"16-21"},"PeriodicalIF":0.0,"publicationDate":"2009-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77763839","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
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