scholarly journals Protocol for the purification of protected carbohydrates: toward coupling automated synthesis to alternate-pump recycling high-performance liquid chromatography

2016 ◽  
Vol 52 (90) ◽  
pp. 13253-13256 ◽  
Author(s):  
Gabe Nagy ◽  
Tianyuan Peng ◽  
Daniel E. K. Kabotso ◽  
Milos V. Novotny ◽  
Nicola L. B. Pohl

Analytical techniques that can be coupled to automated oligosaccharide synthesis platforms are needed to purify to homogeneity protected carbohydrates at levels of ≥99.5% purity.

Author(s):  
Ouakouak Hamza ◽  
Ben Mohamed Moktar ◽  
Ben Chohra Mostafa ◽  
Abdelhamid Zeghdaoui

In this work, we have tried to contribute to the analysis of phenobarbital in the blood. To do this, we used different analytical techniques such as liquid chromatography (HPLC). The results obtained in the course of our work, we can conclude that: The HPLC method was separate phenobarbital endogenous blood components, and optimizing the conditions of chromatographic separation as the composition of the mobile phase consisting of 20% acetonitrile + 20% methanol + 60% ammonium acetate buffer. The extraction with diethyl ether to pH = 4; The chromatographic column, microbondapack ZORBAX C18. A system of diode-array UV detection at 254 nm.


Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2870 ◽  
Author(s):  
Eliza Kurek ◽  
Magdalena Michalska-Kacymirow ◽  
Anna Konopka ◽  
Olga Kościuczuk ◽  
Anna Tomiak ◽  
...  

A fit for purpose analytical protocol was designed towards searching for low molecular weight seleno-compounds in sprouts. Complementary analytical techniques were used to collect information enabling the characterization of selenium speciation. Conceiving the overall characterization of the behavior of selenium, inductively plasma optical mass spectrometry (ICP-MS) was used to determine the total selenium content in entire sprouts as well as in selected extracts or chromatographic fractions. Then, high-performance liquid chromatography combined with ICP-MS (HPLC-ICP-MS) was used to evaluate the presence of inorganic and organic seleno-compounds, with the advantages of being very sensitive towards selenium, but limited by available selenium standard compounds. Finally, ultra-high performance liquid chromatography electrospray ionization triple quadrupole mass spectrometry (UHPLC-ESI-QqQ-MS/MS) and UHPLC-ESI-Orbitrap-MS/MS were used for the confirmation of the identity of selected compounds and identification of several unknown compounds of selenium in vegetable sprouts (sunflower, onion, radish), respectively. Cultivation of plants was designed to supplement sprouts with selenium by using solutions of selenium (IV) at the concentration of 10, 20, 40, and 60 mg/L. The applied methodology allowed to justify that vegetable sprouts metabolize inorganic selenium to a number of organic derivatives, such as seleno-methylselenocysteine (SeMetSeCys), selenomethionine (SeMet), 5′-seleno-adenosine, 2,3-DHP-selenolanthionine, Se-S conjugate of cysteine-selenoglutathione, 2,3-DHP-selenocysteine-cysteine, 2,3-DHP-selenocysteine-cysteinealanine, glutathione-2,3-DHP-selenocysteine, gamma-Glu-MetSeCys or glutamyl-glycinyl-N-2,3-DHP-selenocysteine.


Bioanalysis ◽  
2021 ◽  
Author(s):  
Xiaoyue Shan ◽  
Lei Zhang ◽  
Haipeng Ye ◽  
Ji Shao ◽  
Yanpeng Shi ◽  
...  

Quantification of hippuric acid and methylhippuric acid in human urine matrices provides information on the toluene and xylene exposure conditions. High performance liquid chromatography coupled with UV detection is the preferable technique for hippuric acid and methylhippuric acid detection in human urine. This study was conducted to present analytical techniques developed for monitoring of hippuric acid and methylhippuric acid in human urine matrices during 2016–2021.


Molecules ◽  
2019 ◽  
Vol 24 (6) ◽  
pp. 1119 ◽  
Author(s):  
Chiara Fanali ◽  
Giovanni D’Orazio ◽  
Alessandra Gentili ◽  
Salvatore Fanali

The separation of enantiomers has been started in the past and continues to be a topic of great interest in various fields of research, mainly because these compounds could be involved in biological processes such as, for example, those related to human health. Great attention has been devoted to studies for the analysis of enantiomers present in food products in order to assess authenticity and safety. The separation of these compounds can be carried out utilizing analytical techniques such as gas chromatography, high-performance liquid chromatography, supercritical fluid chromatography, and other methods. The separation is performed mainly employing chromatographic columns containing particles modified with chiral selectors (CS). Among the CS used, modified polysaccharides, glycopeptide antibiotics, and cyclodextrins are currently applied.


Author(s):  
SK MANIRUL HAQUE ◽  
MURAD ALSAWALHA

Amlodipine is the best-prescribed medication for cardiovascular disease major risk factor for hypertension and atorvastatin well known for diabetic. First discussed low cost ultraviolet-visible technique for the determination and quantitation of drugs in pharmaceuticals and biological fluids. Chromatographic techniques have an application with respect to trace analysis. Different types of chromatography such as high-performance liquid chromatography, high performance thin layer chromatography have most frequent applications in the field of pharmaceutical as well as biomedical analyses. Chromatography combined with mass spectrophotometry has the ability to collect molecular ion, followed to prepare a spectrum to assess molecular weight as well as structure. High-performance liquid chromatography coupled with mass spectrophotometry is a reliable and dynamic technique for the analysis of small and large drugs molecule. The advantages and disadvantages of all techniques are compared with each other with respect to sensitivity, reproducibility and other important parameters. The investigation also focused for the quantitation on both drugs in pharmaceutical preparations and plasma samples with the help of all available analytical techniques.


Foods ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 191
Author(s):  
Cristina Cebrián-Tarancón ◽  
José Oliva ◽  
Miguel Ángel Cámara ◽  
Gonzalo L. Alonso ◽  
M. Rosario Salinas

Nowadays, the techniques for the analysis of glycosidic precursors in grapes involve changes in the glycoside structure or it is necessary the use of very expensive analytical techniques. In this study, we describe for the first time an approach to analyse intact glycosidic aroma precursors in grapes by high-performance liquid chromatography with a diode array detector (HPLC-DAD), a simple and cheap analytical technique that could be used in wineries. Briefly, the skin of Muscat of Alexandria grapes was extracted using a microwave and purified using solid-phase extraction combining Oasis MCX and LiChrolut EN cartridges. In total, 20 compounds were selected by HPLC-DAD at 195 nm and taking as a reference the spectrum of phenyl β-D-glucopyranoside, whose DAD spectrum showed a first shoulder from 190 to 230 nm and a second around 200–360 nm. After that, these glycosidic compounds were identified by High-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC-qTOF-MS). Disaccharides hexose pentose were the most abundant group observed with respect to the sugars and monoterpendiols the main aglycones found.


2021 ◽  
Vol 10 (4) ◽  
pp. 3206-3211
Author(s):  
Kishor Danao

Empagliflozin (EMPA), chemically known as (2S,3R,4R,5S,6R)-2-[4-chloro-3-[[4-[(3S)-oxolan-3-yl]oxyphenyl]methyl]phenyl]-6-(hydroxymethyl)oxane-3,4,5-triol is an oral anti-diabetic drug used for treating type 2 diabetes mellitus that produces hypoglycemia by selective and competitive inhibition of sodium/glucose co-transporter-2 (SGLT2) protein. Currently, EMPA is an emerging drug being prescribed by medical practitioners. The quality-oriented scheduled investigation of diverse commercially obtainable formulations of EMPA is a foremost challenge and recently few sophisticated analytical methods are reported for industrial-scale quantitative analysis. Review of analytical method of antidiabetic drug Empagliflozin. This interesting review article covered the recently published sophisticated instruments-based analytical methods in numerous pharmaceutical databases like PubMed, Google Scholar, Science Direct, etc. of diverse areas like spectrophotometry (Ultraviolet-Visible), Ultra-high Performance Liquid Chromatography (UPLC), High-Performance Liquid Chromatography (HPLC), High-Performance Thin Layer Chromatography (HPTLC), and analytical methods for estimation of EPMA in human plasma. From literature, about 19 HPLC methods, 4 UPLC methods, 15 UV-Vis methods, 3 HPTLC methods, and 4 human plasma-based methods were reported for the estimation of EMPA alone or in combination with other drug substances (Linagliptin, Canagliflozin, Dapagliflozin, and Metformin). The methodical insights outlined the reported characteristics like method, detection wavelength, solvent, % recovery, LOD, LOQ, mobile phase composition, flow-rate, column type, retention time, etc. This review concluded that the developed validated analytical methods have a high degree of accuracy, superior reliability, economical to apply, bears good precision, possess better robustness, and greater reproducible attributes which are compulsory features of an ideal method.


Nukleonika ◽  
2016 ◽  
Vol 61 (2) ◽  
pp. 219-223 ◽  
Author(s):  
Krzysztof Kilian ◽  
Zbigniew Rogulski ◽  
Łukasz Cheda ◽  
Agnieszka Drzał ◽  
Marina Gerszewska ◽  
...  

Abstract. A method of automated synthesis of [18F]fluoromisonidazole ([18F]FMISO) for application in preclinical studies on small animals was presented. A remote-controlled synthesizer Synthra RNplus was used for nucleophilic substitution of NITTP (1′-(2′-nitro-1-imidazolyl)-2-O-tetrahydropyranyl-3-O-toluenesulfonyl-propanediol) with 18F anion. Labeling of 5 mg of precursor was performed in anhydrous acetonitrile at 100°C for 10 min, and the hydrolysis with HCl was performed at 100°C for 5 min. Final purification was done with high-performance liquid chromatography (HPLC) and the radiochemical purity of radiotracer was higher than 99%. Proposed [18F]FMISO synthesis was used as a reliable tool in studies on hypoxia in Lewis lung carcinoma (LLC) in mouse models.


2019 ◽  
Vol 7 (1) ◽  
Author(s):  
Ruth Ann Armitage ◽  
Daniel Fraser ◽  
Ilaria Degano ◽  
Maria Perla Colombini

Abstract Yarn samples from the Saltzman Collection of Peruvian dyes were characterized by several different analytical techniques: high performance liquid chromatography with both diode array detection (HPLC-DAD) and electrospray ionisation with tandem mass spectrometry (HPLC-ESI-Q-ToF), direct analysis in real time (DART) mass spectrometry and paper spray mass spectrometry. This report serves primarily as a database of chemical information about the colorants in these dye materials for those studying ancient South American textiles and their colorants. We also provide a comparison of the results obtained by currently widespread HPLC techniques with those of two different ambient ionisation direct mass spectrometry methods to highlight the advantages and disadvantages of these approaches.


Separations ◽  
2021 ◽  
Vol 8 (11) ◽  
pp. 198
Author(s):  
Qian Cheng ◽  
Shuhuan Peng ◽  
Fangyi Li ◽  
Pengdi Cui ◽  
Chunxia Zhao ◽  
...  

Red ginseng (RG) has been extensively utilized in Asian countries due to its pharmacological effects. For the quality evaluation of RG, small molecules, such as ginsenosides, have been widely considered as candidates of its quality markers (Q-markers), and various analytical techniques have been developed in order to identify these compounds. However, despite the efforts to analyze the hydrophobic constituents, it is worth pointing out that about 60% of the mass of RG is made of carbohydrates, including mono-, oligo- and polysaccharides. Consequently, the quality differentiation and identification of RG from the perspective of sugar-markers should be focused. High performance liquid chromatography and evaporative light scattering detector (HPLC–ELSD) method for the determination of disaccharides in RG was established. Furthermore, high performance size exclusion chromatography–multi-angle laser light scattering–refractive index detector (HPSEC–MALLS–RID) for the determination of molecular weight and high performance liquid chromatography photodiode array (HPLC–PDA) for the determination of compositional monosaccharides in RG polysaccharides were also established. HPLC–ELSD/PDA combined with HPSEC–MALLS–RID could be used to determine the contents of disaccharides, molecular weights, and compositional monosaccharides of RG polysaccharides, which could be used for quality control, and this is a new view on the sugar marker to quality differentiation of various origins of RG.


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