Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g-1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

Development and validation of a stability-indicating HPLC method for the determination of buclizine hydrochloride in tablets and oral suspension and its application to dissolution studies

A method using liquid chromatography has been developed and validated for determination of buclizine in pharmaceutical formulations and in release studies. Isocratic chromatography was performed on a C18 column with methanol:water (80:20 v/v, pH 2.6) as mobile phase, at a flow rate of 1.0 mL/min, and UV detection at 230 nm. The method was linear, accurate, precise, sensible and robust. The dissolution test was optimized and validated in terms of dissolution medium, apparatus agitation and rotation speed. The presented analytical and dissolution procedures can be conveniently adopted in the quality and stability control of buclizine in tablets and oral suspension.

Development and validation of a novel stability indicating RP-UPLC method for simultaneous determination of nizatidine, methylparaben and propylparaben in oral liquid pharmaceutical formulation

A selective and accurate stability-indicating gradient reverse phase ultra performance liquid chromatographic method has been developed and validated for the simultaneous determination of nizatidine, methylparaben and propylparaben in pharmaceutical oral liquid formulation. The separation was achieved on Acquity UPLC TM HSS T3 1.8 µm column by using mobile phase containing a gradient mixture of solvent A (0.02 Mol L-1 KH2PO4, pH 7.5) and B (60:40 v/v mixture of methanol and acetonitrile) at flow rate of 0.4 mL min-1. Drug product was exposed to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

Development and validation of a High Performance Liquid Chromatographic method for determination of etoposide in biodegradable polymeric implants

A method using HPLC-UV was developed and validated for the determination of etoposide incorporated into polycaprolactone implants. The method was carried out in isocratic mode using a C18 column (250 x 4.6 mm; 5 µm), at 25 ºC, with acetonitrile and acetic acid 4% (70:30) as mobile phase, a flow rate of 2 mL/min, and UV detection at 285 nm. The method was linear (r² > 0.99) over the range of 5 to 65 µg/mL, precise (RSD < 5%), accurate (recovery of 98.7%), robust, selective regarding excipient of the sample, and had a quantitation limit equal to 1.76 µg/mL. The validated method can be successfully employed for routine quality control analyses.

Development and validation of a dissolution test for primaquine/polyethylene oxide matrix tablets

A simple, precise, specific, repeatable and discriminating dissolution test for primaquine (PQ) matrix tablets was developed and validated according to ICH and FDA guidelines. Two UV assaying methods were validated for determination of PQ released in 0.1 M hydrochloric acid and water media. Both methods were linear (R²>0.999), precise (R.S.D.<1.87%) and accurate (97.65-99.97%). Dissolution efficiency (69-88%) and equivalence of formulations (f2) was assessed in different media and apparatuses (basket/100 rpm and paddle/50 rpm) tested. Discriminating condition was 900 mL aqueous medium, basket at 100 rpm and sampling times at 1, 4 and 8 h. Repeatability (R.S.D.<2.71%) and intermediate precision (R.S.D.<2.06%) of dissolution method were satisfactory.

Transdermal formulations containing human sexual steroids: development and validation of methods and in vitro drug release

In vitro release of bioidentical hormones in four different liposomal transdermal emulsions (containing testosterone, progesterone, estradiol, or estradiol and estriol) was assessed. For this purpose, novel high-performance liquid chromatography methods were developed and validated in an eco-friendly manner and used to determine the in vitro release of such products. The methods were suitable for our intended goal, and the emulsions employed were found to be effective as transporting candidates for the efficient release of hormones in the transdermal delivery of human sexual steroids.

Development and validation of a RP-HPLC method to determine the xanthyletin content in biodegradable polymeric nanoparticles

Xanthyletin is used as an inhibitor of the symbiotic fungus (Leucoagaricus gongylophorus) of the leaf-cutting ant (Atta sexdens rubropilosa), one of the most significant agricultural plague insects. The incorporation of this compound into nanoparticles is a promising approach to effectively control leaf-cutting ants. This study presents the development and validation of a specific analytical method using high-performance liquid chromatography (HPLC) for quantification of the xanthyletin content in biodegradable polymeric nanoparticles. The analytical methodology developed was specific, linear, accurate, precise, and robust. The absolute recovery of xanthyletin in colloidal suspensions was nearly 100%. The HPLC method proved reliable for the quantification of xanthyletin content in nanoparticle formulations.

DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR PALM OIL DETERMINATION IN MICROCAPSULES PRODUCED BY COMPLEX COACERVATION

The microencapsulation of palm oil may be a mechanism for protecting and promoting the controlled release of its bioactive compounds. To optimize the microencapsulation process, it is necessary to accurately quantify the palm oil present both external and internal to the microcapsules. In this study, we developed and validated a spectrophotometric method to determine the microencapsulation efficiency of palm oil by complex coacervation. We used gelatin and gum arabic (1:1) as wall material in a 5% concentration (w/v) and palm oil in the same concentration. The coacervates were obtained at pH 4.0 ± 0.01, decanted for 24 h, frozen (−40 ºC), and lyophilized for 72 h. Morphological analyzes were then performed. We standardized the extraction of the external palm oil through five successive washes with an organic solvent. We then explored the best method for rupturing the microcapsules. After successive extractions with hexane, we determined the amount of palm oil contained in the microcapsules using a spectrophotometer. The proposed method was shown to be of low cost, fast, and easy to implement. In addition, in the validation step, we confirmed the method to be safe and reliable, as it proved to be specific, accurate, precise, and robust.

Development and validation of spectrophotometric method for the determination of DPP-4 inhibitor, sitagliptin, in its pharmaceutical preparations

A simple, sensitive and reproducible spectrophotometric method was developed for the determination of sitagliptin phosphate in bulk and in pharmaceutical formulations. The proposed method is based on condensation of the primary amino group of sitagliptin phosphate with acetyl acetone and formaldehyde producing a yellow colored product, which is measured spectrophotometrically at 430nm. The color was stable for about 1 hour. Beer's law is obeyed over a concentration range of 5-25 µg/ml. The apparent molar absorptivity and Sandell sensitivity values are 1.067 x 10(4) Lmol-1cm-1 and 0.0471 µgcm-2 respectively. All the variables were studied to optimize the reaction conditions. No interference was observed in the presence of common pharmaceutical excipients. The validity of the method was tested by analyzing sitagliptin phosphate in its pharmaceutical preparations. Good recoveries were obtained. The developed method was successfully employed for the determination of sitagliptin phosphate in various pharmaceutical preparations.

Development and validation of spectroscopic methods for simultaneous estimation and dissolution of ofloxacin and ornidazole in tablet dosage forms

The aim of this work was to develop and validate simple, accurate and precise spectroscopic methods (multicomponent, dual wavelength and simultaneous equations) for the simultaneous estimation and dissolution testing of ofloxacin and ornidazole tablet dosage forms. The medium of dissolution used was 900 ml of 0.01N HCl, using a paddle apparatus at a stirring rate of 50 rpm. The drug release was evaluated by developed and validated spectroscopic methods. Ofloxacin and ornidazole showed 293.4 and 319.6nm as λmax in 0.01N HCl. The methods were validated to meet requirements for a global regulatory filing. The validation included linearity, precision and accuracy. In addition, recovery studies and dissolution studies of three different tablets were compared and the results obtained show no significant difference among products.

A Development and Application of a Three-Dimensional Model for a CFB Gasifier

The developing energy markets and rising energy system costs have sparked the need to find new forms of energy production and increase the self-sufficiency of energy production. One alternative is gasification, whose principles have been known for decades, but it is only recently when the technology has become a true alternative. However, in order to meet the requirements of modern energy production methods, it is necessary to study the phenomenon thoroughly. In order to understand the gasification process better and optimize it from the viewpoint of ecology and energy efficiency, it is necessary to develop effective and reliable modeling tools for gasifiers. The main aims of this work have been to understand gasification as a process and furthermore to develop an existing three-dimensional circulating fluidized bed modeling tool for modeling of gasification. The model is applied to two gasification processes of 12 and 50 MWth. The results of modeling and measurements have been compared and subsequently reviewed. The work was done in co-operation with Lappeenranta University of Technology and Foster Wheeler Energia Oy.

Development and characterisation of microsatellite markers for the fungus Lasiodiplodia theobromae

Lasiodiplodia theobromae is an important fungal pathogen of higher plants from tropical and sub-tropical regions. The fungus infects divergent hosts in a wide range of environmental conditions, suggesting that it is highly variable. The aim of this study was to develop new polymorphic microsatellite markers from a Brazilian isolate of L. theobromae that can be used in population studies of this and related fungi. The nine microsatellite markers developed included six that revealed allelic polymorphisms among nine isolates of the disease collected from infected plants in Brazil. Preliminary evaluation of the markers suggested substantial genetic variability among Brazilian L. theobromae populations. These markers have potential utility for evolutionary and epidemiologic studies of this fungus.

A practice perspective on organizational implementation of information technology

Implementering av ett informationssystem ur en organisatorisk synvinkel initieras av en idé om ett system och avslutas då användningen av det inte längre kräver en medveten ansträngning. Ifall tolkningen av implementering är denna, är det fråga om en långsam och komplicerad process, som berör organisationens alla parter. Ny informationsteknologi anses påverka flertalet arbetsprocesser och organiseringen av det dagliga arbetet. Möjligheterna att ta i bruk systemet och utnyttja det är många. I avhandlingen undersöks implementering av ett system för att administrera hemvårdsbesök där hemvårdare använde handdatorer för att registrera information om besökens längd och innehåll. I avhandlingen observeras vilka förändringar som sker i arbetets praxis p.g.a. det nya systemet och hur dessa förändringar påverkar vårdarbetet. Forskningen inleds med att strukturera teorier om arbetspraxis för kommande analys. Arbetspraxis är inarbetade och rutinmässiga arbetssätt i arbetets sociomateriella omgivning. Arbetspraxis i avhandlingen innebär hemvårdarens praxis och upplevd erfarenhet, där verksamheten informeras av gemensamma arbetssätt, projekt, identiteter och intressen. Organisationens auktoritet kommer även fram i den förverkligade arbetspraxisen. Forskningen genomfördes som en etnografisk longitudinell studie under åren 2001-2004. I studien observerades hur nyttjandet av handdatorerna framskred ur ett organisatoriskt perspektiv. Hemvårdares arbete och verksamhet (arbetspraxis) observerades både under vårdsbesök och under pauser. Därtill intervjuades hemvårdarna för att erhålla en bättre förståelse för de rationaliteter som styr arbetet och hur systemet togs i bruk. Dokument relaterade till projektet att införa ett nytt system och administrativa dokument har utnyttjats som källmaterial. Analysen av källmaterialet styrdes av det teoretiska tillvägagångssättet att undersöka arbetspraxis. Problem som identifierades i samband med införandet av systemet och de förändringar som det medförde analyserades i detalj. Parallellt analyserades organisatorisk makt, kontroll och arbetsidentitet. Undersökningen beskriver hur det nya systemet gradvis anpassades till hemvården efter ett initialt motstånd. Under själva implementering av systemet ifrågasattes tidigare arbetspraxis och inställningen till den eftersom arbetspraxisens materiella omgivning förändrades. Det teoretiska tillvägagångssättet i att undersöka arbetspraxis framhäver vårdarens agerande i förändringsprocessen. Resultatet av forskningen visar vikten av realistiska målsättningar, givande av gruppstöd med återkoppling samt förmåga att anpassa sig till det oväntade vid införande av informationssystem.

Consistency and change in Finnish broadcasting policy : the implementation of digital television and lessons from the Canadian experience

Konsistens och förändring i finländsk etermediapolitik. Implementering av digital television och en jämförelse med Kanada Avhandlingen handlar om hur det finländska televisionssystemet förändrades i slutet av 1990-talet från en nationell institution till ett dualistiskt system som präglas av stark marknadsorientering. Syftet med avhandlingen är att förstå på vilket sätt en så snabb förändring kunde ske och analysera de institutionella faktorerna bakom utvecklingen. På teoretisk nivå diskuteras tesen om det nära sambandet mellan statliga politiska institutioner och rundradioverksamhetens institutioner. Avhandlingen består av två fallstudier. Den första sätter fokus på de första åren av den finländska televisionens digitaliseringsprocess som startade med starka industriell-nationalistiska motiveringar. Analysen, som baserar på offentliga dokument, sträcker sig framtill hösten 2001 då de digitala televisionssändningarna startade och regeringspropositionen om den nya kommunikationsmarknadslagen lämnades till riksdagen. Dessa policy-processer analyseras som en ”marknadisering” av de traditionella styrningsprinciper och idéer gällande finländsk rundradioverksamheten. En jämförelse mellan Finlands och Kanadas nationella rundradiopolitik gör att man kan koppla slutsatserna till den internationella utvecklingen. Jämförelsen visar hur kommunikationspolitiska linjen i de två länderna har kommit att likna varandra trots att ländernas tv-system och deras styrordningar är mycket olika. Exemplet med Kanada visar att den särskilda teknologin inte är viktig utan snarare de kommersiella intressen som står bakom och som beslutsfattare gärna döljer i en nationalistisk retorik. Studien visar att det är viktigt att beakta vilken tyngd man i politiken ger de två sidor som rundradioverksamheten består av: sändningsteknologin och verksamheten som en speciell kulturform. Nationalstatens handlingsutrymme minskar inom fältet om målet är att vara framgångsrik i konkurrensen i den nya internationella ekonomin. Enligt de nyliberalistiska principer som det politiska systemet överlag har tillägnat sig det är önskvärd men också helt inhemska institutionella traditioner och praxis som följdes i den finländska digitaliseringsprocessen främjade utvecklingen som ledde till att nästan alla ursprungliga nationella syften föll sönder.