Quantification of beta-lactam antibiotics in veterinary drugs: amoxicillin and ampicillin determination by high performance liquid chromatography

This work focused on the development and validation of an RP-HPLC-UV method for quantification of beta-lactam antibiotics in three pharmaceutical samples. Active principles analyzed were amoxicillin and ampicillin, in 3 veterinary drugs. Mobile phase comprised 5 mmol L-1 phosphoric acid solution at pH 2.00, acetonitrile with gradient elution mode and detection wavelength at 220 nm. The method was validated according to the Brazilian National Health Surveillance regulation, where linear range and linearity, selectivity, precision, accuracy and ruggedness were evaluated. Inter day precision and accuracy for pharmaceutical samples 1, 2 and 3 were: 1.43 and 1.43%; 4.71 and 3.74%; 2.72 and 1.72%, respectively, while regression coefficients for analytical curves exceeded 0.99. The method had acceptable merit figure values, indicating reliable quantification. Analyzed samples had active principle concentrations varying from -12 to +21% compared to manufacturer label claims, rendering the medicine unsafe for administration to animals.

Preparative separation of C19-diterpenoid alkaloids from Aconitum carmichaelii Debx by pH‑zone-refining counter-current chromatography

The technique of pH-zone-refining counter-current chromatography was successfully applied to preparatively separate three C19-diterpenoid alkaloids from the crude extracts of Aconitum carmichaelii for the first time using a two-phase solvent system of petroleum ether-ethyl acetate-methanol-water (5:5:1:9, v/v/v/v). Mesaconitine (I), hypaconitine (II), and deoxyaconitine (III) were obtained from 2.5 g of the crude alkaloids in a one-step separation; the yields were 4.16%, 16.96%, and 5.05%, respectively. The purities of compounds I, II, and III were 93.0%, 95%, and 96%, respectively, as determined by HPLC. The chemical structures of the three compounds were identified by electrospray ionization mass spectrometry (ESI-MS) and NMR.

Inovação & propriedade industrial & indústria química

ABSTRACT The main aim of this paper was to contribute to reflections in Brazil on the need to transfer knowledge held at universities and R&D institutions over to companies, i.e. to transfer scientific knowledge of chemistry to technology. It discusses how the competitiveness of countries is increasingly dependent on their technological capacity. The chemicals industry is a fundamental driver of social, environmental, economic and industrial indicators of sustainable development. In Brazil, the chemicals industry's deficit has grown over the last three decades. Patents are important sources of information because patent documents contain 75% of all technological information available. The National Institute of Industrial Property in Brazil has created a Technology Observatory with the purpose of identifying and analyzing technological information contained in patent documents within the ambit of partnerships with government entities or business associations, in order to support their technology-related decision-making processes. The paper gives examples of ethanol and biotechnology patent documents, including pharmaceuticals, of which there are very few in Brazil. However, a few of the patent applications identified are filed in Brazil, giving the country the opportunity to transform this scientific knowledge into technology by means of partnership agreements with companies. Finally, the paper presents information on the patent applications filed by the world's leading chemicals companies as measured by their revenues, and the respective numbers of patent applications in the last five years in organic chemistry and polymers, sectors in which Brazil is currently dependent on imports for over 50% of its needs. The patent assignees in these sectors in Brazil are also identified, and the paper concludes that Brazil needs to invest in the development of professionals, providing clearly-defined career paths in technology innovation teams at R&D institutions, and to foster more initiatives such as the creation of a new research and innovation entity, EMBRAPII, since investing in science and technology is a prerequisite for knowledge production, industrial property, economic development and, consequently, the competitiveness of the country.

Super/subcritical fluid chromatography with packed columns: state of the art and applications

Separations using supercritical fluid chromatography (SFC) with packed columns have been re-discovered and explored in recent years. SFC enables fast and efficient separations and, in some cases, gives better results than high performance liquid chromatography (HPLC). This paper provides an overview of recent advances in SFC separations using packed columns for both achiral and chiral separations. The most important types of stationary phases used in SFC are discussed as well as the most critical parameters involved in the separations and some recent applications.

Separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography

An effective method for the rapid separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography (HSCCC) was successfully established. In the present study, a two-phase solvent system composed of chloroform-n-butanol-methanol-water (4:1:4:2, v/v/v/v) was used for HSCCC separation. A one-step separation in 4 h from 150 mg of crude extract produced 26.3 mg of trans-resveratrol-3-O-glucoside, 42.0 mg of pieceid-2"-O-gallate, and 17.9 mg of trans-resveratrol with purities of 99.1%, 97.8%, and 99.4%, respectively, as determined by high-performance liquid chromatography (HPLC). The chemical structures of these compounds were identified by nuclear magnetic resonance (NMR) spectroscopy.

Application of fourier transform infrared spectroscopy, chemical and chemometrics analyses to the characterization of agro-industrial waste

Agroindustrial waste in general presents significant levels of nutrients and organic matter and has therefore been frequently put to agricultural use. In this context, the objective of this study was to determine the chemical composition, nitrogen, phosphorus, potassium, calcium, magnesium and carbon content, as well as the qualitative characteristics through Fourier transform infrared spectroscopy of four samples of poultry litter and one sample of cattle manure, from the southwestern region of Paraná, Brazil. Results revealed that, in general, the poultry litter presented higher amount of nutrients and carbon than the cattle manure. The infrared spectra allowed identification of the functional groups present and the differences in degree of sample humification. The statistical treatment confirmed the quantitative and qualitative differences revealed.

DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

Ilex paraguariensis (yerba-mate) is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD) model and ultra high-performance liquid chromatography (UHPLC). The presence of these three phytochemical markers in the extracts was evaluated using UHPLC-MS and was confirmed by the chromatographic bands in the total ion current traces (m/z of 181.1 [M+H]+, 195.0 [M+H]+, and 353.0 [M−H]−, respectively). The developed method was then transferred to a high-performance liquid chromatography (HPLC) platform, and the three phytochemical markers were used as external standards in the validation of a method for analyses of these compounds in extracts using a diode array detector (DAD). The validated method was applied to quantify the chlorogenic acid, caffeine, and theobromine in the samples. HPLC-DAD chromatographic fingerprinting was also used in a multivariate approach to process the entire data and to separate the I. paraguariensis extracts into two groups. The developed method is very useful for qualifying and quantifying I. paraguariensis extracts.

Improving demand forecasting practices in the industrial context

Demand forecasting is one of the fundamental managerial tasks. Most companies do not know their future demands, so they have to make plans based on demand forecasts. The literature offers many methods and approaches for producing forecasts. When selecting the forecasting approach, companies need to estimate the benefits provided by particular methods, as well as the resources that applying the methods call for. Former literature points out that even though many forecasting methods are available, selecting a suitable approach and implementing and managing it is a complex cross-functional matter. However, research that focuses on the managerial side of forecasting is relatively rare. This thesis explores the managerial problems that are involved when demand forecasting methods are applied in a context where a company produces products for other manufacturing companies. Industrial companies have some characteristics that differ from consumer companies, e.g. typically a lower number of customers and closer relationships with customers than in consumer companies. The research questions of this thesis are: 1. What kind of challenges are there in organizing an adequate forecasting process in the industrial context? 2. What kind of tools of analysis can be utilized to support the improvement of the forecasting process? The main methodological approach in this study is design science, where the main objective is to develop tentative solutions to real-life problems. The research data has been collected from two organizations. Managerial problems in organizing demand forecasting can be found in four interlinked areas: 1. defining the operational environment for forecasting, 2. defining the forecasting methods, 3. defining the organizational responsibilities, and 4. defining the forecasting performance measurement process. In all these areas, examples of managerial problems are described, and approaches for mitigating these problems are outlined.

Controle da requeima em tomateiro industrial com fungicidas e silicato de potássio

O objetivo deste trabalho foi avaliar o efeito da aplicação de fungicidas e silicato de potássio, no controle da requeima (Phytophthora infestans), em tomateiro industrial. Os fungicidas foram aplicados com base no sistema de previsão de Wallin e calendário fixo de pulverizações. Empregou-se o delineamento em blocos casualizados com 6 tratamentos e 4 repetições. Os tratamentos (T) foram: T1 - testemunha; T2 - dimetomorfe + clorotalonil (valores de severidade da doença (VSD = 10) + metiram; T3 - metalaxil-M + clorotalonil (VSD = 10) + metiram (o metiram foi aplicado somente na semana onde o VSD não atingiu o valor requerido para o tratamento); T4 - calendário fixo: dimetomorfe + clorotalonil, mancozeb, metalaxil-M + clorotalonil e clorotalonil, alternados semanalmente; T5 - silicato de potássio (5 g/L) e T6 - silicato de potássio (15 g/L). A severidade foi avaliada utilizando-se uma escala descritiva variando de 0 a 100 %. A severidade final foi: 100; 2,6; 12,3; 5,5; 97,6 e 96 %, respectivamente, nos tratamentos T1, T2, T3, T4, T5 e T6. A severidade foi em média, 93 % menor nos tratamentos que receberam aplicações de fungicidas em relação a testemunha. Dentre os tratamentos que empregaram sistema de previsão o 2 apresentou melhor resultado do que o 3. O tratamento 2 apresentou eficiência comparável ao calendário semanal (tratamento 4), apresentando produtividades de 62.103,73 e 52.473,33 kg/ha, respectivamente, sendo superiores aos demais tratamentos. Aplicações de silicato de potássio nas duas doses testadas não diferiram significativamente da testemunha, indicando a ineficiência do produto em controlar a requeima.

Segmentation of Industrial Customers – Case: Finnish Mechanical Engineering Companies

Segmentointi on perinteisesti ollut erityisesti kuluttajamarkkinoinnin työkalu, mutta siirtymä tuotteista palveluihin on lisännyt segmentointitarvetta myös teollisilla markkinoilla. Tämän tutkimuksen tavoite on löytää selkeästi toisistaan erottuvia asiakasryhmiä suomalaisen liikkeenjohdon konsultointiyritys Synocus Groupin tarjoaman case-materiaalin pohjalta. K-means-klusteroinnin avulla löydetään kolme potentiaalista markkinasegmenttiä perustuen siihen, mitkä tarjoamaelementit 105 valikoitua suomalaisen kone- ja metallituoteteollisuuden asiakasta ovat maininneet tärkeimmiksi. Ensimmäinen klusteri on hintatietoiset asiakkaat, jotka laskevat yksikkökohtaisia hintoja. Toinen klusteri koostuu huolto-orientoituneista asiakkaista, jotka laskevat tuntikustannuksia ja maksimoivat konekannan käyttötunteja. Tälle kohderyhmälle kannattaisi ehkä markkinoida teknisiä palveluja ja huoltosopimuksia. Kolmas klusteri on tuottavuussuuntautuneet asiakkaat, jotka ovat kiinnostuneita suorituskyvyn kehittämisestä ja laskevat tonnikohtaisia kustannuksia. He tavoittelevat alempia kokonaiskustannuksia lisääntyneen suorituskyvyn, pidemmän käyttöiän ja alempien huoltokustannusten kautta.

Isolation of lignans glycosides from Alibertia sessilis (Vell.) K. Schum. (Rubiaceae) by preparative high-performance liquid chromatography

Enantiomeric aglycone lignans contained in a mixture were separated from a fraction of the extract of the stems of Alibertia sessilis (Vell.) K. Schum. (Rubiaceae) by preparative high-performance liquid chromatography. An efficient and fast separation can be achieved with methanol-water (30:70, v/v). Their structures were identified as (+)-lyoniresinol 3alpha-O-beta-glucopyranoside and (-)-lyoniresinol 3alpha-O-beta-glucopyranoside, being reported for the first time in Rubiaceae.

Use Of Systems Approach with Total Quality Management in Industrial Organizations

The objective of the work has been to study why systems thinking should be used in combination with TQM, what are the main benefits of the integration and how it could best be done. The work analyzes the development of systems thinking and TQM with time and the main differences between them. The work defines prerequisites for adopting a systems approach and the organizational factors which embody the development of an efficient learning organization. The work proposes a model based on combination of an interactive management model and redesign to be used for application of systems approach with TQM in practice. The results of the work indicate that there are clear differences between systems thinking and TQM which justify their combination. Systems approach provides an additional complementary perspective to quality management. TQM is focused on optimizing operations at the operational level while interactive management and redesign of organization are focused on optimization operations at the conceptual level providing a holistic system for value generation. The empirical study demonstrates the applicability of the proposed model in one case study company but its application is tenable and possible also beyond this particular company. System dynamic modeling and other systems based techniques like cognitive mapping are useful methods for increasing understanding and learning about the behavior of systems. The empirical study emphasizes the importance of using a proper early warning system.

Developing the service offering of an industrial company

The purpose of this thesis was to determine, what kind of service offering the case company should provide to its customers in the Australian market. For this, a model for analysing the competitive environment was developed. In the model, three players were considered: customers, competitors and the case company. Benchmarking was used in identifying competitors’ offerings currently available in the market. Experts inside the case company were consulted for determining the customer need. The competitors’ offerings were analysed on the basis of Pekkarinen et al.’s (2009) framework, dividing the offerings to services supporting the supplier’s product (SSP), supporting the client (SSC), supporting the client’s network (SSN), supporting mutual actions (SSM) and benefit and risk sharing elements. After this, they were compared to the competitive environment in order to identify areas where the case company can differentiate itself from its competitors in the Australian market. On the basis of the company’s key success factors, and the Finnish service concept currently in use, some additional offerings were suggested for the case company in order to further outperform its competitors in the market. Finally, on the basis of the suggested offerings and competitors’ offerings, a service concept was suggested for the case company to introduce in the Australian market.

Manejo da requeima do tomateiro industrial empregando sistema de previsão

Três experimentos foram conduzidos utilizando-se o híbrido de tomateiro industrial H 7155N, em 2003 e 2004 visando adequar um sistema de previsão modificado para o uso de fungicidas no manejo da requeima causada por Phytophthora infestans. Os experimentos foram conduzidos num delineamento em blocos ao acaso com dez tratamentos e três repetições. Os fungicidas sistêmicos foram aplicados quando o valor de severidade da doença (VSD) alcançou oito, dez ou doze pontos. A alternância dos fungicidas sistêmicos com o metiram ocorreu na semana em que não foram alcançados os VSD´s. O tratamento calendário de pulverização para o controle da requeima consistiu da aplicação semanal de fungicidas após o aparecimento dos primeiros sintomas e aqueles definidos pelo sistema de previsão foram baseados nos VSD acumulados durante o experimento. A avaliação da requeima foi feita semanalmente com auxílio de uma escala descritiva de severidade e uma chave diagramática. A eficiência dos tratamentos foi comparada calculando-se a área abaixo da curva do progresso da doença, a taxa de progresso da doença (r) e produtividade de tomate. Os valores de r do melhor tratamento (dimetomorfe misturado com clorotalonil (VSD = 10) alternado com metiram variaram de 0,03 a 0,07, enquanto para o tratamento calendário semanal foi de 0,05 a 0,09 e para testemunha de 0,24 a 0,39. Dimetomorfe + clorotalonil (VSD = 10) alternado com metiram produziu em média 15,7 toneladas a mais de tomate, comparado ao tratamento calendário semanal de fungicidas. Dimetomorfe ou metalaxil-M misturado com clorotalonil (VSD = 10) baseado no sistema de previsão sem a alternância com metiram diferiu do calendário semanal baseado na severidade da doença e na produção de tomate. Os tratamentos piraclostrobina misturado com metiram (VSD = 8; VSD = 10) alternado com metiram; dimetomorfe misturado com mancozeb (VSD = 8; VSD = 10) alternado com metiram proporcionaram controle intermediário da requeima. O sistema de previsão baseado no uso de dimetomorfe misturado com clorotalonil alternado com metiram (VSD = 10) permitiu redução de uma aplicação da mistura dimetomorfe misturado com clorotalonil pulverização em dois dos três experimentos, comparados ao tratamento calendário semanal de aplicação de fungicidas, sem afetar a produção.

Determinants of cash holdings in Finnish industrial sector: measuring the impact of financial crisis 2007- 2010

This thesis studies cash and short term investments to net assets ratio of Finnish industrial companies during financial crisis, and how different firm specific and macro economical variables affect cash and short term investments. The data consists of quarter level interim reports. Regression analysis was used to find out the effects of different variables. Regression models were formed based on previous studies on cash holdings. It was found that firms studied held more cash during financial crisis than before it. Cash and short-term investments acted as substitute of net working capital. Leverage had a positive and significant relationship to cash and short term investment ratio. It was also found out that firms have a target cash and short term investments ratio.