Determination of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy

A simple analytical method for quantification of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy is described. The method is based on the reaction, on the filter paper surface, between the drug and p-chloranil producing a colored compound. The best reaction conditions were obtained with 20 µL of atenolol solution and 20 µL of p-chloranil. All reflectance measurements were carried out at 550 nm and the linear range was from 1.13x10-2 to 7.88x10-2 mol L-1 (r = 0.9992). The limit of detection was 2.80 x 10-3 mol L-1. The proposed method was successfully applied to analysis of different commercial brands of pharmaceutical formulations and the results obtained by the proposed method were in good agreement with those obtained using the British Pharmacopoeia method.

Spectrophotometric determination of metronidazole through Schiff's base system using vanillin and PDAB reagents in pharmaceutical preparations

Two simple sensitive and reproducible spectrophotometric methods have been developed for the determination of metronidazole either in pure form or in their tablets. The proposed methods are based on the reduction of the nitro group to amino group of the drug. The reduction of metronidazole was carried out with zinc powder and 5 N hydrochloric acid at room temperature in methanol. The resulting amine was then subjected to a condensation reaction with aromatic aldehyde namely, vanillin and p-dimethyl amino benzaldehyde (PDAB) to yield yellow colored Schiff's bases. The formed Schiff's bases are quantified spectrophotometrically at their absorption maxima at 422 nm for vanillin and 494 nm for PDAB. Beer's law was obeyed in the concentration ranges 10 to 65 µg mL-1 and 5 to 40 µg mL-1 with a limit of detection (LOD) of 0.080 µg mL-1 and 0.090 µg mL-1 for vanillin and PDAB, respectively. The mean percentage recoveries were found to be 100.05 ± 0.37 and 99.01 ± 0.76 for the two methods respectively. The proposed methods were successfully applied to determine the metronidazole in their tablet formulations and the results compared favorably to that of reference methods. The proposed methods are recommended for quality control and routine analysis.

Potentiometric determination of Minoxidil in topical use pharmaceutical samples

A potentiometric titration method for the determination of minoxidil based on its redox reaction with K2Cr2O7 is described. The best results were observed using 1.00 x 10-3 mol L-1 K2Cr2O7 and 1.00 x 10-2 mol L-1 minoxidil solutions, and the minoxidil as titrant in 2.00 mol L-1 H2SO4 medium. The method was applied to commercial samples and compared with the results from a chromatographic procedure. Recoveries from 97.4 to 98.7 % were observed depending on the sample. Comparison with the chromatographic procedure reveled agreement within 90% confidence level.

Sensitive spectrophotometric determination of lamotrigine in bulk drug and pharmaceutical formulations using bromocresol green

Two new, simple, rapid and reproducible spectrophotometric methods have been developed for the determination of lamotrigine (LMT) both in pure form and in its tablets. The first method (method A) is based on the formation of a colored ion-pair complex (1:1 drug/dye) of LMT with bromocresol green (BCG) at pH 5.02±0.01 and extraction of the complex into dichloromethane followed by the measurement of the yellow ion-pair complex at 410 nm. In the second (method B), the drug-dye ion-pair complex was dissolved in ethanolic potassium hydroxide and the resulting base form of the dye was measured at 620 nm. Beer's law was obeyed in the concentration range of 1.5-15 µg mL-1 and 0.5-5.0 µg mL-1 for method A and method B, respectively, and the corresponding molar absorptivity values are 1.6932 x 10(4) and 3.748 x 10(4) L mol-1cm-1. The Sandell sensitivity values are 0.0151 and 0.0068 µg cm-2 for method A and method B, respectively. The stoichiometry of the ion-pair complex formed between the dug and dye (1:1) was determined by Job's continuous variations method and the stability constant of the complex was also calculated. The proposed methods were applied successfully for the determination of drug in commercial tablets.

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.

A simple spectrophotometric method for the determination of captopril in pharmaceutical preparations using ammonium molybdate

A simple, rapid and sensitive spectrophotometric method for the determination of captopril (CPT) in pharmaceutical formulations is proposed. This method is based on the reduction reaction of ammonium molybdate, in the presence of sulphuric acid, for the group thiol of CPT, producing a green compound (λ max 407 nm). Beer's law is obeyed in a concentration range of 4.60 x 10-4 - 1.84 x 10-3 mol l-1 of CPT with an excellent correlation coefficient (r = 0.9995). The limit of detection and limit of quantification were 7.31 x 10-6 e 2.43 x 10-5 mol l-1 of CPT, respectively. The proposed method was successfully applied to the determination of CPT in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the official reported method at 95 % confidence level.

Apteekkien kannattavuuden kehittäminen toimintolaskentaa soveltaen

Apteekkiliiketoiminta eroaa tavallisesta liiketoiminnasta erilaisten lakisääteisten velvoitteiden vuoksi. Alan regulaation viimeaikainen kehitys, kuten lääkevaihto, viitehintajärjestelmä sekä näiden tuoma lääkkeiden tiukentunut hintakilpailu, ovat tuoneet haasteita apteekkien kannattavuuteen. Tuotevalikoima- ja varastonhallinta ovat nousseet yhä tärkeämpään rooliin. Tutkimuksen tavoitteena oli kehittää apteekkien kannattavuutta toimintolaskentaa soveltaen. Toimintolaskennalla kahdelle apteekille tuotettiin kustannus- sekä tuotekannattavuustietoa. Tutkimuksen teoreettinen viitekehys koostui toimintolaskennan sekä apteekkiliiketoiminnan aikaisemmasta tutkimuksesta. Tutkimuksesta kävi ilmi, että kummassakin apteekissa oli erittäin laaja tuotesortimentti. Itsehoito- sekä vapaan kaupan tuotteiden tuotesortimenttia järkeistämällä kannattavuutta voitaisiin parantaa. Monesti tuotekategorioissa on useita saamaa vaikuttavaa ainetta sisältävää valmistetta usealta eri toimittajalta mikä heikentää kannattavuutta. Tuloksista kävi ilmi myös, että tulevaisuudessa vapaan kaupan tuotteet tulevat olemaan tärkeässä roolissa, mikä korostaa markkinointi- ja myyntiosaamisen tärkeyttä. Reseptilääkkeissä kate ei näyttäisi kattavan kustannuksia, minkä vuoksi varastonhallintaan on kiinnitettävä huomiota.

Potentiometric and conductimetric studies of chemical equilibria for pyridoxine hydrochloride in aqueous solutions: simple experimental determination of pKa values and analytical applications to pharmaceutical analysis

The combination of two low-cost classical procedures based on titrimetric techniques is presented for the determination of pyridoxine hydrochloride in pharmaceuticals samples. Initially some experiments were carried out aiming to determine both pKa1 and pKa2 values, being those compared to values of literature and theoretical procedures. Commercial samples containing pyridoxine hydrochloride were electrochemically analysed by exploiting their acid-base and precipitation reactions. Potentiometric titrations accomplished the reaction between the ionizable hydrogens present in pyridoxine hydrochloride, being NaOH used as titrant; while the conductimetric method was based on the chemical precipitation between the chloride of pyridoxine hydrochloride molecule and Ag+ ions from de silver nitrate, changing the conductivity of the solution. Both methods were applied to the same commercial samples leading to concordant results when compared by statistical tests (95 and 98% confidence levels). Recoveries ranging from 99.0 to 108.1% were observed, showing no significant interference on the results.

Packaging concept development for an assortment of medical device products

Diplomityön tavoitteena oli kehittää Wipak Oy:n valmistamille sterilointipakkauksille tulevaisuuden pakkauskonsepti. Sterilointipakkaukset luokitellaan lääkelaitedirektiivin mukaan lisätarvikkeiksi luokan 1 lääkelaitteille, ja tämä näkökulma oli vahvasti mukana konseptin kehityksessä. Lähtökohtana pakkauskonseptin suunnittelulle oli tuotteiden arvoketjussa, eli pakata tuotteet siten että pakkausten avulla voidaan tuottaa lisäarvoa arvoketjun toimijoille. Tavoitteena oli parantaa pakkausten viestintää, toimivuutta/tehokkuutta toimitusketjussa sekä vahvistaa brändin imagoa myynti- ja kuljetuspakkauksen avulla. Lääkinnälliset laitteet ja tarvikkeet ovat lainsäädännön ja normien avulla tarkasti säädeltyjä. Näiden normien vaatimukset asettavat perusteet myynti- ja kuljetuspakkausten kehittämiselle. Tämän lisäksi suunnittelussa on huomioitu asiakkaiden toiveet ja kehitystarpeet. Kirjallisuusosuudessa on keskitytty lääkinnällisten laitteiden pakkausyksiköiden toimintoihin sekä niiden kehitysnäkymiin. Pääpaino on ollut pakkausmerkintöjen ja jäljitettävyyden kehittämisellä, koska tietojen automaattisen tunnistuksen hyödyntäminen lääkintälaitteiden pakkausten arvoketjussa on kasvava trendi. Manuaalisesti tehtävät tuotevirtojen kirjaukset ketjun eri toimijoiden osalta lisäävät riskejä jäljitettävyyden kannalta ja aiheuttavat lisätyötä ja – kustannuksia ketjun kaikille osapuolille. Ehdotus uudesta pakkauskonseptista on kehitetty näiden tietojen pohjalta. Ehdotuksessa on huomioitu lainsäädännöstä ja ketjun toimijoilta tulevat tarpeet, sekä alan tulevaisuuden kehitysnäkymät. Ehdotetun pakkauskonseptin avulla saadaan lisättyä myynti- ja kuljetuspakkausten tehokkuutta, parannettua jäljitettävyyttä ja helpotettu arvoketjun alavirran toimijoiden työtä lisäämällä erillinen sisäpakkaus myyntiyksikön sisälle. Työssä on lisäksi selvitetty pakkauskonseptin kustannusvaikutukset tuotteiden hintaan. Lopussa on ehdotettu jatkotoimenpiteet suunnitelman implementoimisesta käytäntöön.

Market entry patterns of Finnish SMEs entering China

In 2011 China became the world’s second largest economy overtaking Japan. With its rapidly growing middle class buying diverse goods from consumption products to sophisticated technology and luxury products, it is also the fastest growing export market in the world. The purpose of this study is to examine what types of market entry modes Finnish SMEs use in China, which factors affect on their decisions and whether they have switched or combined the strategies after entering China. The goal is to understand the relevance of the entry mode choice related to the internationalization process and to evaluate how well it suits the Chinese business environment. The empirical part of the study is a semi structured qualitative analysis of six case companies that represent different industry fields. The cases were selected based on the recent literature about the Finnish industry fields China is interested in to gain knowledge and expertise from. Companies included in the study are an architect office, two pharmaceutical development companies, an ICT company, a plastic mechanics company and a clean tech company. The results of this study indicated that the market entry patterns of Finnish SMEs in China differ from each other based on the factors related to company’s background, mode concerns and Chinese market influences.

Control system for forced-air cooling of horticultural products

This work is a study of the implementation of a classical controller using a tuning method referred to as IMC (Internal Model Control) and aimed at the reduction of electrical energy consumption by the appropriate relation between energy consumption and the cooling time with forced air. The supervisory system installed was able to manipulate the variable of frequency of the signal power of the exhaust fan engine (forced air module), to accelerate or decelerate the loss of heat from the product to be cooled by airflow variation that passes through the mass of the produce. The results demonstrated a reduction in energy consumption from 64% and an increase of only 8% in the cooling time to the system using PI/IMC (Proportional - Integral with IMC) tuning method compared with the system in its operating nominal condition. This PI/IMC control may be implemented directly in a frequency converter, without the need to purchase a computer or PLC (programmable logic controller) to run the dedicated application, increasing its economical viability.

Seasonality of net radiation in two sub-basins of Paracatu by the use of modis sensor products

The net radiation (Rn) represents the main source of energy for physical and chemical processes that occur in the surface-atmosphere interface, and it is used for air and soil heating, water transfer, in the form of vapor from the surface to the atmosphere, and for the metabolism of plants, especially photosynthesis. If there is no record of net radiation in certain areas, the use of information is important to help determine it. Among them we can highlight those provided by remote sensing. In this context, this work aims to estimate the net radiation, with the use of products of MODIS sensor, in the sub-basins of Entre Ribeiros creek and Preto River, located between the Brazilian states of Goiás and Minas Gerais. The SEBAL (Surface Energy Balance Algorithm for Land) was used to obtain the Rn in four different days in the period of July to October, 2007. The Rn results obtained were consistent with others cited in the literature and are important because the orbital information can help determine the Rn in areas where there are not automatic weather stations to record the net radiation.

Development of simple and efficient synthetic strategies for production of fine chemicals of pharmaceutical relevance : metal-mediated allylation combined with applied catalysis

Den snart 200 år gamla vetenskapsgrenen organisk synteskemi har starkt bidragit till moderna samhällens välfärd. Ett av flaggskeppen för den organiska synteskemin är utvecklingen och produktionen av nya läkemedel och speciellt de aktiva substanserna däri. Därmed är det viktigt att utveckla nya syntesmetoder, som kan tillämpas vid framställningen av farmaceutiskt relevanta målstrukturer. I detta sammanhang är den ultimata målsättningen dock inte endast en lyckad syntes av målmolekylen, utan det är allt viktigare att utveckla syntesrutter som uppfyller kriterierna för den hållbara utvecklingen. Ett av de centralaste verktygen som en organisk kemist har till förfogande i detta sammanhang är katalys, eller mera specifikt möjligheten att tillämpa olika katalytiska reaktioner vid framställning av komplexa målstrukturer. De motsvarande industriella processerna karakteriseras av hög effektivitet och minimerad avfallsproduktion, vilket naturligtvis gynnar den kemiska industrin samtidigt som de negativa miljöeffekterna minskas avsevärt. I denna doktorsavhandling har nya syntesrutter för produktion av finkemikalier med farmaceutisk relevans utvecklats genom att kombinera förhållandevis enkla transformationer till nya reaktionssekvenser. Alla reaktionssekvenser som diskuteras i denna avhandling påbörjades med en metallförmedlad allylering av utvalda aldehyder eller aldiminer. De erhållna produkterna innehållende en kol-koldubbelbindning med en närliggande hydroxyl- eller aminogrupp modifierades sedan vidare genom att tillämpa välkända katalytiska reaktioner. Alla syntetiserade molekyler som presenteras i denna avhandling karakteriseras som finkemikalier med hög potential vid farmaceutiska tillämpningar. Utöver detta tillämpades en mängd olika katalytiska reaktioner framgångsrikt vid syntes av dessa molekyler, vilket i sin tur förstärker betydelsen för de katalytiska verktygen i organiska kemins verktygslåda.

Fractionation of Hen Egg and Oat Lipids with supercritical Fluids Chemical and functional Properties of Fractions

Hen eggs and oats (Avena Sativa) are important materials for the food industry. Today, instead of merely satisfying the feeling of hunger, consumers are asking for healthier, biologically active and environmentally friendly products. The growing awareness of consumers’ increasing demands presents a great challenge to the food industry to develop more sustainable products and utilise modern and effective techniques. The modification of yolk fatty acid composition by means of feed supplements is well understood. Egg yolk phospholipids are polar lipids and are used in several applications including food, cosmetics, pharmaceuticals, and special nutrients. Egg yolk phospholipids are excellent emulsifiers, typically sold as mixtures of phospholipids, triacylglycerols, and cholesterol. However, highly purified and characterised phospholipids are needed in several sophisticated applications. Industrial fractionation of phospholipids is usually based on organic solvents. With these fractionation techniques, some harmful residues of organic solvents may cause problems in further processing. The objective of the present study was to investigate the methods to improve the functional properties of eggs, to develop techniques to isolate the fractions responsible for the specific functional properties of egg yolk lipids, and to apply the developed techniques to plant-based materials, too. Fractionation techniques based on supercritical fluids were utilised for the separation of the lipid fractions of eggs and oats. The chemical and functional characterisation of the fractions were performed, and the produced oat polar lipid fractions were tested as protective barrier in encapsulation processes. Modifying the fatty acid compositions of egg yolks with different types of oil supplements in feed had no affect on their functional or sensory properties. Based on the results of functional and sensory analysis, it is evident that eggs with modified fatty acid compositions are usable in several industrial applications. These applications include liquid egg yolk products used in mayonnaise and salad dressings. Egg yolk powders were utilised in different kinds of fractionation processes. The precipitation method developed in this study resembles the supercritical anti-solvent method, which is typically used in the pharmaceutical industry. With pilot scale supercritical fluid processes, non-polar lipids and polar lipids were successfully separated from commercially produced egg yolk powder and oat flakes. The egg and oat-based polar lipid fractions showed high purities, and the corresponding delipidated fractions produced using supercritical techniques offer interesting starting materials for the further production of bioactive compounds. The oat polar lipid fraction contained especially digalactosyadiacylglycerol, which was shown to have valuable functional properties in the encapsulation of probiotics.