Diss. (sammanfattning) Uppsala : Uppsala universitet, 2005. / Härtill 6 uppsatser.

Diss. (sammanfattning) Uppsala : Sveriges lantbruksuniv., 2007. / Härtill 7 uppsatser.

Class of 2012 Abstract / Specific Aims: To assess the chemical stability of ampicillin for injection in normal saline at pH values ranging from 5 to 6. Methods: A stability-indicating high performance liquid chromatography (HPLC) method was developed and used to determine the stability of ampicillin for injection in normal saline following buffering with sodium acetate and acid adjustment with HCl at pH values of 5, 5.5, and 6. To confirm that the assay was stability-indicating, ampicillin trihydrate reference standard (1 mg/mL) was exposed to alkali, acid, and oxidative stress conditions and analyzed by HPLC for the presence of degradation products. Analysis was performed on a reverse-phase (C-18) column with a mobile phase consisting of water, acetonitrile, 1 M monobasic potassium phosphate, and 1 N acetic acid (909:80:10:1). Other HPLC parameters were: flow rate 1 mL/min; detection wavelength 254 nm; injection volume 20 µL; column temperature 30˚C. The method was evaluated for linearity, precision, and accuracy. The chemical stability of ampicillin for injection (18 mg/mL) in normal saline and sodium acetate (pH adjusted at values of 5, 5.5, and 6) was assessed at baseline (t=0), 7, 11, 17, 31, and 44 hours and compared to a control solution (no pH adjustment). Measurements at each time interval were performed in triplicate. Main Results: Ampicillin trihydrate reference standard (1 mg/mL) was adequately separated from degradation products following exposure to alkali, acid, and oxidative stress conditions. After 16 hours, a precipitate was observed in the solution at pH 6, and therefore stability is not reported. All other solutions (pH 5, pH 5.5, and control) were stable for at least 24 hours at room temperature and yielded t90 values of 110, 64.2, and 27.5 hours, respectively. Conclusions: Adjustment of intravenous ampicillin solutions to pH values of 5 or 5.5 significantly increased stability. Ampicillin appears to be most stable at a pH near its isoelectric point (pH 5).

Charles University in Prague Pharmaceutical Faculty in Hradec Králové Department of Pharmaceutical Botany and Ecology Candidate: Miloslava Ďuráčová Consultant: RNDr. Jitka Vytlačilová, Ph.D. Title of thesis: HPLC-MS determination of active biological compounds in Elbe river Biologically active compounds have a various ways to enter environment. They can occur as pesticides, cosmetics and pharmaceutics and their metabolites. Such compounds are classified as environmental contaminants. There is a increased environmental concentration connected with increasing consumption of biologically active compounds. There is a urgent need to follow the effect on the different parts of ecosystem and levels of biologically active compounds. This work was prepared during the cooperation with Povodí Labe state enterprise. A novel analytical method was described in the experimental part of this thesis. I was employed to evaluate biologically compounds levels in the surface water samples. This method is now routinely used. 10 out of 19 evaluated compounds reached concentrations higher than LOD. Acetaminophene (559 ng/l, Králický stream), gabapentine (457 ng/l Elbe, LB Schmilka), cotinine (139 ng/l, Králický potok) were the biologically active compounds with the highest found concentrations. Keywords: HPLC-MS analysis,...

Propolis is an approved food additive containing flavonoids as a major active constituent. Variability has been found in the composition of propolis in distinctive regions and it was noticed that there are limitations in the analysis of propolis. In this study, the identification of ten flavonoids and residual antibiotics in propolis was investigated by using several liquid chromatography techniques, including reversed-phase high-performance liquid chromatography (RP-HPLC), microemulsion LC (MELC) and ultra-performance LC (UPLC). The ten flavonoids that were selected for this research include rutin, myricetin, quercetin, apigenin, kaempferol, pinocembrin, CAPE, chrysin, galangin and acacetin while chlortetracycline, oxytetracycline and doxycycline were selected to examine the residual antibiotics in propolis. For the analysis of the selected flavonoids, routine RP-HPLC method was found to be the best method, while MELC technique was found more efficient for the analysis of the selected antibiotics. Solid phase extraction with HLB sorbent was utilised in the analysis of antibiotics for clean-up of propolis. In method development studies for flavonoids and antibiotics, one-factor-at-a-time (OFAT) approach was followed. The final optimised method for the analysis of flavonoids as well as the method. for the analysis of antibiotics was validated using the ICH guidelines, and various aspects, such as the linearity, selectivity, accuracy, recovery, robustness and stability parameters, were examined. Development of efficient conventional method for the extraction of flavonoids from propolis was studied extensively in the present research work using different extraction techniques such as maceration, hot extraction, ultrasound assisted extraction. Among all extraction experiments, ethanolic extraction using ultrasound extraction method was the best efficient approach. This thesis shows that, in general, the performance of O/W MELC is superior to that of conventional HPLC for the determination of residual antibiotics in propolis. UPLC was not suitable for the analysis of flavonoids and antibiotics. The conventional LC was the only technique to separate the ten flavonoids but MELC was able to separate nine of the flavonoids with faster analysis time. This work also showed that MELC uses cheaper solvents. This considerable saving in both cost and time will potentially improve efficiency within quality control.

Zirconia is one of the most promising column packing materials for High Performance Liquid Chromatography (HPLC). The perfect HPLC support material should be energetically homogenous, have a high surface area on which different chemical species can reversibly attach and be physically and chemically stable over a wide range of pH, temperature and solvent conditions. Most existing supports do not have all of these properties. This project is also focused on a proteomics study. Zirconia, hafnium oxide and titanium oxide which are some of the more promising materials currently available, can be used for the separation and analysis of phosphorylated proteins. Adenosine triphosphate, Adenosine diphosphate and Adenosine monophosphate were used as prototypes for phosphorylated proteins. Separation, absorption, fluorescence and SEM studies were performed to determine the adsorption of Adenosine phosphates species at a particular pH on Zirconia. Zirconia was also used for the purification of Fibrinogen Growth Factor (FGF) protein, which are a family of growth factors involved in angiogenesis, wound healing, and embryonic development. The sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) technique was used to analyze the off-column purification and separation of this protein. This research suggests that, at acidic conditions, adenosine monophosphate has more favorable absorption on the Zirconia surface. On the other hand, the separation study suggests that basic conditions are more favorable for the absorption of ATP, ADP and AMP when mixed together on Zirconia 500. Furthermore, it was found that Zirconia is a very promising material for the purification of FGF protein.

In natural dendroflora of Lithuania willow genus (Salix L.) is abundant in species amount. Its bark contains active materials which are known as possessing anti-inflammatory properties since former times. Bark extracts are contained in analgesic as well as antirheumatic preparations. Its therapeutic effectiveness is associated with salicine which turns into salicylic acid. Willow bark is a know phytotherapeutic precursor of aspirin. To use more natural and not synthetic materials in the 21st century the methods for extraction of active materials for medicine are being sought. Thus, the studies on plant groups possessing the most intense anti-inflammatory properties became urgent. The amount of salicin varies among different species. Acording to the European Pharmacopoea, minimal amount of 1,5% of salicin is required in Willow bark. The aim of the study was to investigate salicylates amount variation in willow bark of different Salix species growing in Lithuania. The studies were carried out using the routine methods of pharmacopeia. After extraction analysis was performed by high performance liquid chromatography (HPLC) method. The first step of study was made among 3 samples of each plant, colected at different growing period (1-st year autumn, 2-nd year autumn and 2-nd year spring). Comparison of the quantities of the salicylic derivatives depending upon age of the plant and time of collection shows, that plants at two years of growth and collected in autumn accumulate... [to full text] / Natūralioje Lietuvos floroje gluosnių (Salix L.) rūšys yra plačiai paplitusios. Gluosnio žievė – nuo seno žinoma kaip priešuždegiminiu poveikiu pasižyminti vaistinė augalinė žaliava. Jos ekstraktai įeina į priešreumatinių ir analgezinių preparatų sudėtį. Terapinis veikimas yra susijęs su salicinu, kuris organizme virsta salicilo rūgštimi. Gluosnio žievė yra fitoterapinis aspirino pirmtakas. XXI amžiuje vis didesnis dėmesys krypsta į natūralius, o ne sintetinius preparatus. Tokiu būdu, augalų, pasižyminčių terapinėmis savybėmis tyrimai įgyja didelę reikšmę. Skirtingų rūšių gluosnių žievėje, kaupiamas salicino kiekis skiriasi. Europos farmakopėjoje reglamentuojamas minimalus salicino kiekis yra 1,5%. Šio tyrimo tikslas buvo Ištirti Lietuvoje augančių gluosnio rūšių salicilatų kiekio įvairavimą vaistinėje augalinėje žaliavoje (žievėje). Darbo uždaviniai- atlikti įvairių Lietuvoje augančių gluosnio rūšių salicilatų kiekio analizę, palyginti salicilatų kiekį gluosnio žievėje, atsižvelgiant į augalo amžių bei rinkimo laiką bei įvertinti gautus rezultatus, numatomą terapinį veikimą. Tyrimai atlikti naudojant farmakopėjinius analizės metodus. Žievės ekstraktai buvo tiriami efektyviosios skysčių chromatografijos metodu.Šio tyrimo pirmo etapo metu išanalizuota 12 gluosnių taksonų. Buvo ištirti vienerių ir dviejų metų, taip pat pavasarį ir rudenį rinkti žievės pavyzdžiai. Didesni kiekiai aktyvių medžiagų rasta rudenį ir 2 metų amžiaus gluosnių žievės pavyzdžiuose. Antrajame tyrimo... [toliau žr. visą tekstą]

Orientador: Adriana Zerlotti Mercadante / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-19T23:50:04Z (GMT). No. of bitstreams: 1 Ceresino_ElaineBerger_M.pdf: 1060543 bytes, checksum: 13a878710ce1aecca57313b218a6eb55 (MD5) Previous issue date: 2012 / Resumo: Os pigmentos naturais, entre os quais se destacam antocianinas e carotenóides, proporcionam cor aos alimentos. A cor percebida é considerada um fator de qualidade e um atributo fundamental na aceitação e escolha de um alimento. Em paralelo, estes pigmentos também possuem importantes funções biológicas, sendo considerados promotores da saúde humana. A araçaúna (Psidium eugeniaefolia) é uma fruta de cor roxa, de sabor exótico e mede até 3 cm de diâmetro, encontrada na região da Mata Atlântica, desde o Estado do Espírito Santo até o Rio Grande do Sul. Por se tratar de uma fruta pouco pesquisada objetivo do presente trabalho foi caracterizar e quantificar as antocianinas e os carotenóides. A composição de carotenóides e de antocianinas foi determinada em três lotes de araçaúna coletados no município de Santa Maria de Jetibá, Estado do Espírito Santo. Os lotes apresentaram em média entre 3,0 e 3,2 mg/g de antocianinas, entre as quais se destaca cianidina 3- glucosídeo (74%). Em relação aos carotenóides, o conteúdo variou entre 30,0 e 35,4 µg/g, sendo os carotenóides majoritários a luteína (49-53%), seguido de ß-caroteno (13%). Esses pigmentos foram separados, identificados e quantificados por cromatografia líquida de alta eficiência acoplada a um detector de arranjo e diodos e espectrômetro de massas (HPLC-DAD-MS/MS) / Abstract: The natural pigments, mainly anthocyanins and carotenoids, promote color to food. The perceived color is considered a factor of quality and a key attribute of acceptance and choice of this food. Additionally, these pigments also present remarkable biological functions and are considered promoters of the human health. Araçaúna (Psidium eugeniaefolia) is a purple fruit, presenting an exotic flavor and it is up to 3 cm in diameter. They are found in the Atlantic Forest region, from Espírito Santo State to Rio Grande do Sul State, Brazil. Taking in consideration that few reports are found in literature about this fruit, the aim of this work was to characterize and quantify anthocyanins and carotenoids. The composition of carotenoids and anthocyanins were determined in three batches of araçaúna collected from Santa Maria de Jetibá, Espirito Santo State. The batches presented concentration between of 3.0 and 3.2 mg/g (dry basis) of anthocyanins, where cyanidin 3 - glucoside was the major one (74%). Regarding the carotenoid content, it ranged between 30.0 and 35.4 mg/g (dry basis), where the main carotenoids were lutein (49-53%), followed by ß-carotene (13%). These pigments were separated, identified and quantified by high performance liquid chromatography coupled to a diode array detector and tandem mass spectrometer (HPLC-DAD-MS/MS) / Mestrado / Ciência de Alimentos / Mestre em Ciência de Alimentos

Antibiotics are widely used pharmaceuticals in human and veterinary medicine. These compounds are biologically active. They decrease efficiency of biological processes in wastewater treatment plants. Antibiotics are not eliminated from sewage water completely and they are discharged as contaminants into the receiving waters. Several methods exist for the determination of antibiotics in sewage water. In the first place liquid chromatography, gas chromatography and capillary electrophoresis are used. The aim of this thesis was to developed a suitable izolation technique and an optimal analytical method for identification and determination of penicillins in wastewater. For determination was selected amoxicillin, ampicillin and benzylpenicillin (penicillin G). These are very often used penicillins. An optimized method was used for determination of these penicilins in real samples from a wastewater treatment plant situated in Veterinary and pharmaceutical university in Brno and from the large-scale wastewater treatment plant in Brno-Modřice. Real samples were concentrated using SPE (solid phase extraction). For penicillins determination were used high performance liquid chromatography with diode array detection (HPLC/DAD).

The PhD thesis deals with determination of sulfonamides and tetracyclines in waste waters. Sulphonamides and tetracyclines are widely used in human and veterinary medicine. They are biologically active compounds and block biological processes in waste water treatment plants. These substances can influence microorganisms in the environment. Sulphonamides and tetracyclines induce resistance in low concentrations. These substances penetrate into the environment from industrial production, use in households, hospitals, veterinary clinics and fish farms. Tetracyclines and sulphonamides were determined in waste water from waste water treatment plants in Brno. Optimalization of extraction of these compounds was performed by solid phase extraction. Sulphonamides and tetracyclines were determined by liquid chromatography coupled with diode array detector or coupled with mass spectrometry. Optimalized method was used for determination tetracyclines and sulphonamides in waste water from waste water treatment plants in Brno in years 2007 – 2010.