Lyotropic behavior of Gelucire 50/13 by XRD, Raman and IR spectroscopies according to hydration.

The present paper discuss the structural and vibrational properties of polyoxyethylene glycol glycerides (Gelucire 50/13) during the hydration with increasing water from 0% to 80%. The Gelucire 50/13 used as sustained release matrix forming agent in pharmaceutical applications and it was essentially studied by Small and Wide Angle X-ray Scattering (SWAXS), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy according to the rate of hydration. The hydration behavior of this amphiphilic excipient has been investigated in the spectral range 4000-0cm-1 in Raman spectroscopy, and 4000-600cm-1 in FTIR. At increasing water contents Gelucire 50/13 forms successive bicontinuous to micellar supramolecular structures, and the vibrational changes were directly correlated with this conformational changes of the Gelucire structure. Overall, Raman and IR spectroscopy clearly demonstrated that the different functional groups studied could be characterized independently, allowing for the understanding of their role in Gelucire polymorphism.

Validación y acreditación de procedimientos analíticos de macronutrientes: aplicación al análisis nutricional en purés de dietas geriátricas / Validation and accreditation of analytical procedures of macronutrients: application to nutritional analysis in purées of geriatric diets

ANTECEDENTES Y OBJETIVOS: Al objeto de asegurar la calidad en la determinación de macronutrientes de las conservas de raciones de combate del Ejército de Tierra y de platos cocinados, se realiza la validación y acreditación de los procedimientos analíticos, y se aplican al análisis nutricional de purés, pertenecientes a dietas geriátricas de una Residencia Militar de Atención a Mayores de la Dirección de Asistencia al Personal del Ejército de Tierra. MATERIAL Y MÉTODOS: Los ensayos se realizan con procedimientos analíticos internos. La estimación de la incertidumbre se realiza según los principios de la guía EURACHEM/CITAC. RESULTADOS: Rango de valores en ensayos de materiales de referencia certificados (MRC): HUMEDAD: sesgo relativo, 0,19-3,86%; DERR 0,31-1,76%; DERr 0,25-0,86%; HORRATr 0,15-0,72; Urel 1,67-9,80%. PROTEÍNA: sesgo relativo, 0,00-2,17 %; DERR, 0,77-5,79 %; DERr , 0,34-2,94 %; HORRATr, 0,34-1,44; Urel 1,66-18,3%. Límite de detección (LD), 0,08% de nitrógeno. Límite de cuantificación (LC), 0,29 % de nitrógeno. CENIZAS: sesgo relativo, 2,50-13,63%; DERR, 2,42-16,62%; DERr , 0,62-8,26%; HORRATr, 0,65-3,30; Urel 6,86-45,7%. GRASA: sesgo relativo, 3,74-5,88%; DERR 0,98-3,32%; DERr 0,94-3,22%; HORRATr 0,34-1,36%; Urel 13,0-15,8%. En los ensayos de aptitud se obtiene un Z-score z≤ 2. Las 51 muestras de purés, elaborados de forma culinaria, arrojan los siguientes valores medios, en porcentaje: humedad (81,3±4,0); proteína (5,17±2,14); grasa (3,15±1,27); cenizas (0,98±0,48). CONCLUSIONES: Los procedimientos analíticos son útiles en el rango de determinación. El alcance de la acreditación (ENAC, España) afecta a humedad (40-95%); proteína (0,5-46%), grasa (3,5-50%) y cenizas (0,4-4%)

BACKGROUNDS AND OBJECTIVES: In order to ensure the quality in determining macronutrients in canned foods of combat rations Spanish Army and cooked dishes, validation and accreditation of analytical procedures are carried out. These are applied to nutritional analysis in purées of geriatric diets of a Military Old People's Home of the Direction of Personal Assistance Spanish Army. MATERIAL AND METHODS: Assays were performed with internal analytical procedures. The uncertainty estimation is performed according to the principles of EURACHEM/CITAC guide. RESULTS: Value range of assays of certified reference materials (CRMs): MOISTURE: relative bias, 0,19- 3,86%; RSDR 0,31-1,76%; RSDr 0,25-0,86%; HORRATr 0,15-0,72; Urel 1,67-9,80%. PROTEIN: relative bias, 0,00-2,17 %; RSDR, 0,77-5,79 %; RSDr , 0,34-2,94 %; HORRATr, 0,34-1,44; Urel 1,66-18,3%. Limit of detection (LOD), 0,08% of nitrogen. Limit of quantitation (LOQ), 0,29 % of nitrogen. ASH: relative bias, 2,50-13,63%; RSDR, 2,42-16,62%; RSDr , 0,62-8,26%; HORRATr, 0,65-3,30; Urel 6,86-45,7%. FAT: relative bias, 3,74-5,88%; RSDR 0,98-3,32%; RSDr 0,94-3,22%; HORRATr 0,34-1,36%; Urel 13,0-15,8%. Proficiency testing exercices got a Z-score z≤ 2. The analysis of 51 purées samples, elaborated in a culinary form, yield the following mean values in percent: moisture (81,3±4,0); protein (5,17±2,14); fat (3,15±1,27); ash (0,98±0,48). CONCLUSIONS: The analytical procedures are useful within the range of determination. The reach of accreditation (ENAC, Spain) affects moisture (40-95%); protein (0,5-46%), fat (3,5-50%) and ash (0,4-4%)

Lauric fat cocoa butter replacer from krabok (irvingia malayana) seed fat and coconut oil.

Lauric fat cocoa butter replacer (LCBR) was produced from a blend of krabok seed fat (KSF) and coconut oil (CO). Four fat blends with different ratios of KSF/CO (20/80, 40/60, 60/40 and 80/20 (%wt)), CO, KSF and a commercial LCBR (C-LCBR) were characterized using various techniques. It was found that blend 60/40 exhibited SFC curve and crystallization/melting behavior most similar to that of C-LCBR. The blend met the requirements to be considered as LCBR and has potential as an alternative to commercial LCBR that are being used nowadays and hence it was recommended as LCBR (called R-LCBR). The polymorphic behavior of both C-LCBR and R-LCBR was investigated and both fats displayed mainly short spacing pattern associated with ß' polymorph, a required polymorph for LCBR. The compatibility between R-LCBR and CB was investigated by mixing the R-LCBR with CB in different proportions and softening due to the eutectic effect was observed in the mixed fats. This limits the proportion of CB and the R-LCBR in compound coatings to no more than 5% of CB in the total fat phase.

Enzymatic synthesis of extra virgin olive oil based infant formula fat analogues containing ARA and DHA: one-stage and two-stage syntheses.

Structured lipids (SLs) with high palmitic acid content at the sn-2 position enriched with arachidonic acid (ARA) and docosahexaenoic acid (DHA) were produced using extra virgin olive oil, tripalmitin, ARA and DHA single cell oil free fatty acids. Four types of SLs were synthesized using immobilized lipases, Novozym 435 and Lipozyme TL IM, based on one-stage (one-pot) and two-stage (sequential) syntheses. The SLs were characterized for fatty acid profile, triacylglycerol (TAG) molecular species, melting and crystallization profiles, tocopherols, and phenolic compounds. All the SLs had >50 mol % palmitic acid at the sn-2 position. The predominant TAGs in all SLs were PPO and OPO. The total tocopherol content of SL1-1, SL1-2, SL2-1, and SL2-2 were 70.46, 68.79, 79.64, and 79.31 µg/g, respectively. SL1-2 had the highest melting completion (42.0 °C) and crystallization onset (27.6 °C) temperatures. All the SLs produced in this study may be suitable as infant formula fat analogues.

Medium chain and behenic acid incorporated structured lipids from sal, mango and kokum fats by lipase acidolysis.

Medium chain (MC) and behenic fatty acids were incorporated into kokum, sal and mango fats using 1,3-specific lipase catalysed acidolysis. The incorporation of fatty acids increased with increase in concentration of fatty acids and duration of reaction. The order of incorporation of fatty acids was C22:0>C10:0>C8:0, to the extent of 53%, 42.5%, 35.8%, respectively, after 16 h, using kokum as substrate. The same trend was observed with sal or mango fats as substrates though the percentages incorporated were different. The modified products with higher contents of MC were liquids with no solid fats, even at 0°C, and which showed low cloud point due to an increase in triacylglycerols containing lower chain fatty acids. The modified products after incorporating both MC and C22:0 showed long melting ranges and were suitable for use in bakery, confectionery, etc. as vanaspati substitutes.

Crystallization of fully hydrogenated and interesterified fat and vegetable oil.

Owing to public concern regarding the adverse health effects of trans fatty acids, an alternative technology to trans fats has recently become an important issue. The interesterification of fully hydrogenated vegetable oil and liquid oil blends is one of the most versatile options. This paper reports a physical analysis of high-melting fat (HMF) prepared through the interesterification of fully hydrogenated soybean oil and regular soybean oil, and through fractionation. The thermal and structural properties of the HMF blended with salad oil at a mass ratio of 4:1 (called the HMF blend, hereafter), which was prepared as a model fat blend for margarine, were assessed using X-ray diffraction (XRD), differential scanning calorimetry (DSC), and polarized light microscopy (POM). To observe the polymorphic transformation, all samples were aged after crystallization, and the development of granular crystals during the aging process was observed. We found that the granular crystals are made of SOS/SSO, POS/PSO, and (SOS+POS)/(SSO+PSO) molecular compounds, all of which easily transform into ß form with a double-chain-length structure.

Conversion of olive pomace oil to cocoa butter-like fat in a packed-bed enzyme reactor.

Refined olive pomace oil (ROPO) was utilized as a source oil for production of cocoa butter-like fat. Immobilized sn-1,3 specific lipase catalyzed acidolysis of ROPO with palmitic (PA) and stearic (SA) acids was performed in a laboratory scale packed-bed reactor. Effect of reactor conditions on product formation was studied at various substrate mole ratios (ROPO:PA:SA; 1:1:1, 1:1:3, 1:3:3, 1:2:6), enzyme loads (10%, 20%, 40%), substrate flow rates (1.5, 4.5, 7.5, 15 ml/min) and solvent amounts (150, 400 ml). The highest yield (10.9% POP, 19.7% POS and 11.2% SOS) was obtained at 40% enzyme load, 1:2:6 substrate mole ratio, 45 degrees C, 7.5 ml/min substrate flow rate, 150 ml solvent and 3h reaction time. The melting profile and SFC of the product were comparable to those of CB. Polarized light microscope (PLM) images showed no drastic changes in polymorphic behavior between CB and product.