DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR ISOSULFAN BLUE BY LIQUID CHROMATOGRAPHY

Objective: To develop and validate new, simple and rapid analytical method for determination of related impurities in isosulfan blue drug substances by the liquid chromatographic method as per ICH guidelines.Methods: The chromatographic separation obtained between drug substance i.e. isosulfan blue and its related impurities (Impurity-A, Impurity-B and Impurity-C) on C18 (100 x 2.00 mm) 1.9µ UPLC column using a mobile phase system containing 0.1 % perchloric acid in water (Mobile phase A) and 0.1 % perchloric acid in mixture of 30 volumes of water and 70 volumes of acetonitrile (Mobile Phase B) with gradient program; detector wavelength 220 nm and column temperature 30 °C. The developed method was extensively validated according to ICH guidelines.Results: Good linearity was observed for isosulfan blue, impurity-A, impurity-B and impurity-C, linearity was calculated from loq Level To 150%with respect to specification level. The correlation coefficient R = 0.999 was proved and showed that the method is robust. The limit of detection of isosulfan blue, impurity-A, impurity-B and impurity-C were found to be 0.010%, 0.015%, 0.030% and 0.0075 % respectively and limit of quantitation of isosulfan blue, impurity-A, impurity-B and impurity-C were found to be 0.030%, 0.030%, 0.045% and 0.015% respectively for 2ml injection volume. The percentage recovery of isosulfan blue and its related impurities were ranged from 94.0 to 108.0 in bulk drug samples. Isosulfan blue sample solution and mobile phase were found to be stable for at least 72 h. The proposed method was found to be suitable and accurate for the quantitative determination of impurity-A, impurity-B, impurity-C and other unknown impurities in isosulfan blue drug substances.Conclusion: A new, simple and rapid method has been developed and validated for separation and determination of impurity-A, impurity-B, impurity-C and unknown impurities of isosulfan blue by the reverse-phase liquid chromatographic method. Analytical method was developed and validated as per ICH guidelines.The developed method can be used for the quantitative determination of impurity A, impurity B, impurity C and unknown impurities in isosulfan blue drug substances in pharmaceutical industry

ENANTIOMERIC SEPARATION OF ETODOLAC IN A BULK DRUG SUBSTANCE BY REVERSE-PHASE CHIRAL LIQUID CHROMATOGRAPHY METHOD

Objective: To develop novel, simple and rapid enantiomeric separation of Etodolac by reverse-phase high-performance liquid chromatographic method as per ICH guidelines.Methods: The R-isomer and S-isomer were baseline resolved on a CHIRAL-AGP, (100 x 4.0 mm i. d, 5 mm) column using a mobile phase system containing 0.1 M sodium dihydrogen phosphate dihydrate pH 4.0 buffer: Isopropanol (85:15 v/v.) at detector wavelength 225 nm and column temperature 25 °C. The chromatographic resolutions between R-isomer and S-isomer were found three. The developed method was extensively validated according to ICH guidelines.Results: Good linearity was observed for R-isomer over the concentration range of 300–3000 ng/ml, with the linear regression (Correlation coefficient R = 0.999) and proved to be robust. The limit of detection and limit of quantification of R-isomer was found to be 300 and 900 ng/ml, respectively for 10 ml injection volume. The percentage recovery of R-isomer was ranged from 98.0 to 102.0 in bulk drug samples of Etodolac. Etodolac sample solution and mobile phase were found to be stable for at least 48 hours. The proposed method was found to be suitable and accurate for the quantitative determination of R-isomer in bulk drugs.Conclusion: A novel, simple and rapid enantiomeric separation of Etodolac by reverse-phase high-performance liquid chromatographic method was developed and validated as per ICH guidelines. The developed method can be used for the quantitative determination R-isomer in bulk drug materials in pharmaceutical industry.Â

SEPARATION AND DETERMINATION OF THE S-ISOMER OF (10-CAMPHORSULFONYL) OXAZIRIDINE IN A BULK DRUG SUBSTANCE BY NORMAL-PHASE LIQUID CHROMATOGRAPHY

Objective: To develop novel, simple and accurate enantiomeric separation of (10-Camphorsulfonyl) oxaziridine by normal-phase high-performance liquid chromatographic method as per ICH guidelines.Methods: The S-isomer and R-isomer of (10-Camphorsulfonyl) oxaziridine were baseline resolved on a Chiralcel OD-H (250 x 4.0 mm i. d, 5 mm) column using a mobile phase system containing n-Hexane: ethanol: trifluoroacetic acid (90:10:0.1 v/v/v.) at detector wavelength 210 nm and column temperature 30 °C. The chromatographic resolutions between S-isomer and R-isomer were found three. The developed method was extensively validated according to ICH guidelines.Results: Good linearity was observed for S-isomer over the concentration range of 900–9000 ng/ml, with the linear regression (Correlation coefficient R = 0.999) and proved to be robust. The limit of detection and limit of quantification of S-isomer was found to be 400 and 900 ng/ml, respectively for 20 ml injection volume. The percentage recovery of S-isomer was ranged from 97.0 to 102.0 in bulk drug samples of (10-Camphorsulfonyl) oxaziridine. (10-Camphorsulfonyl) oxaziridine sample solution and mobile, phase was found to be stable for at least 48 hours. The proposed method was found to be suitable and accurate for the quantitative determination of S-isomer in bulk drugs.Conclusion: A novel, simple and accurate normal phase LC method was described for the enantiomeric separation of 10-Camphorsulfonyl Oxaziridine is precise and specific.Â

Optimisation of granola breakfast cereal manufacturing process by wet granulation and pneumatic conveying

This study has considered the optimisation of granola breakfast cereal manufacturing processes by wet granulation and pneumatic conveying. Granola is an aggregated food product used as a breakfast cereal and in cereal bars. Processing of granola involves mixing the dry ingredients (typically oats, nuts, etc.) followed by the addition of a binder which can contain honey, water and/or oil. In this work, the design and operation of two parallel wet granulation processes to produce aggregate granola products were incorporated: a) a high shear mixing granulation process followed by drying/toasting in an oven. b) a continuous fluidised bed followed by drying/toasting in an oven. In high shear granulation the influence of process parameters on key granule aggregate quality attributes such as granule size distribution and textural properties of granola were investigated. The experimental results show that the impeller rotational speed is the single most important process parameter which influences granola physical and textural properties. After that binder addition rate and wet massing time also show significant impacts on granule properties. Increasing the impeller speed and wet massing time increases the median granule size while also presenting a positive correlation with density. The combination of high impeller speed and low binder addition rate resulted in granules with the highest levels of hardness and crispness. In the fluidised bed granulation process the effect of nozzle air pressure and binder spray rate on key aggregate quality attributes were studied. The experimental results show that a decrease in nozzle air pressure leads to larger in mean granule size. The combination of lowest nozzle air pressure and lowest binder spray rate results in granules with the highest levels of hardness and crispness. Overall, the high shear granulation process led to larger, denser, less porous and stronger (less likely to break) aggregates than the fluidised bed process. The study also examined the particle breakage of granola during pneumatic conveying produced by both the high shear granulation and the fluidised bed granulation process. Products were pneumatically conveyed in a purpose built conveying rig designed to mimic product conveying and packaging. Three different conveying rig configurations were employed; a straight pipe, a rig consisting two 45° bends and one with 90° bend. Particle breakage increases with applied pressure drop, and a 90° bend pipe results in more attrition for all conveying velocities relative to other pipe geometry. Additionally for the granules produced in the high shear granulator; those produced at the highest impeller speed, while being the largest also have the lowest levels of proportional breakage while smaller granules produced at the lowest impeller speed have the highest levels of breakage. This effect clearly shows the importance of shear history (during granule production) on breakage during subsequent processing. In terms of the fluidised bed granulation, there was no single operating parameter that was deemed to have a significant effect on breakage during subsequent conveying. Finally, a simple power law breakage model based on process input parameters was developed for both manufacturing processes. It was found suitable for predicting the breakage of granola breakfast cereal at various applied air velocities using a number of pipe configurations, taking into account shear histories

Benefits of Value Addition in Agricultural Produce on Land, Water and Labor Productivities under Arid Agriculture: Case of Dates in Oman

Oman is an arid country in the Middle East with water scarcity, and hence land and labor management issues hindering agricultural sustainability and food security. Value addition can minimize food wastes, which is crucial to achieve sustainability by improving the land, water and labor productiveness. This study aimed to evaluate and quantify the improvements in land, water and labor productivities through value addition in date cultivated under arid conditions in Oman. Five date factories and different value-added products of the most popular date varieties, Khalas and Fardh were selected for this study. The comparisons were made between productivity improvements of the value-added products and the raw products. Khalas dates value-added with nuts had the highest productivity ratio of 540%, the same for Fardh was 360% while the lowest were in Khalas value-added with flavors with 111% and in Fardh date paste with 129%. In Khalas, the best improvement by the value addition in average land, water and labor productivities from the base-values of 6.93 ton ha-1, 0.57 kg m-3, and 0.82 kg h-1 of the raw date were 25.05 ton ha-1, 2.06 kg m-3, and 2.95 kg h-1 in date with nuts, respectively; while in the Fardh, these were 18.82 ton h-1, 1.55 kg m-3, and 2.21 kg h-1 respectively of the same value-added product. The variations in productivity improvement of selected value-added products could be due to the availability and cost of the raw dates, cost of the value addition, market options and selling price. Value addition showed high potential for improving productivities under arid conditions and is worth making adoption efforts for achieving agricultural sustainability goals

Effect of pretreatment and temperature on drying characteristics and quality of green banana peel

In banana cultivation, a considerable amount of the production is wasted every year because of various constraints present in the post-harvest management chain. Converting green banana pulp and peels into flour could help to reduce losses and enable the food sector to keep the product for an entire year or more. In order to use green banana fruit and peel flour in the food industry as a raw ingredient such as in bakery and confectionery items—namely biscuits, cookies, noodles, nutritious powder, etc.—it is essential to standardize the process for the production of the flour. As a result, the purpose of this study was to investigate the influence of pretreatment and temperature on the drying capabilities and quality of dried green banana peel. The green banana peel pieces were pretreated with 0.5 and 1.0% KMS (potassium metabisulfite), and untreated samples were taken as control, and dried at 40°, 50°, and 60 °C in a tray dryer. To reduce the initial moisture content of 90–91.58% (wb) to 6.25–9.73% (wb), a drying time of 510–360 min was required in all treatments. The moisture diffusivity (Deff) increased with temperature, i.e., Deff increased from 5.069–6.659 × 10−8, 6.013–7.653 × 10−8, and 4.969–6.510 × 10−8 m2/s for the control sample, 0.5% KMS, and 1.0% KMS, respectively. The Page model was determined to be the best suited for the drying data with the greatest R2 and the least χ2 and RSME values in comparison with the other two models. When 0.5% KMS-pretreated materials were dried at 60 °C, the water activity and drying time were minimal. Hue angle, chroma, and rehydration ratio were satisfactory and within the acceptable limits for 0.5% KMS-pretreated dried banana peel at 60 °C

Modification of secondary craters on the Martian South Polar Layered Deposits

Secondary crater fields are important stratigraphic markers that can shed light on resurfacing processes that have occurred since their formation. We examine the morphologies of secondary craters formed from the ejection of material from two large impacts on the Martian South Polar Layered Deposits (SPLD): McMurdo crater at 84.5°S, 0°W, and an unnamed impact at 80.8°S, 284°W. The morphologies of these secondary craters allow us to impose constraints on the modification history of the SPLD. We have quantified crater morphologies using data sets from the Mars Global Surveyor and Mars Odyssey missions. We find a complete lack of secondary craters smaller than 300 m in diameter in both crater fields, which implies that at least the upper 30 m of the deposits have been resurfaced since the time of these impacts. Secondary crater depth-to-diameter ratios are low (average of 0.016), indicating that significant degradation has occurred since their emplacement. We find that vertical resurfacing alone is not enough to explain the observed depth-to-diameter distribution and suggest that viscous relaxation of craters coupled with a small amount of vertical resurfacing best fits the data. In the McMurdo field, high depth-to-diameter craters are found preferentially on steeper terrain associated with scarps cutting through the secondary field. This observation suggests that crater modification exhibits a dependence on slope. We comment on possible mechanisms that may explain this observation. The morphologies of secondary craters on the SPLD point to modification processes without lunar parallel and not yet fully modeled for Mars

Design of Packaging Vents for Cooling Fresh Horticultural Produce

Abstract This review focuses on the design of vents in packages used for handling horticulture produce. The studies on vent designs that are conducted to obtain fundamental understanding of the mechanisms by which different parameters affect the rate and homogeneity of the airflow and the cooling process are presented. Ventilated packages should be designed in such a way that they can provide a uniform airflow distribution and consequently uniform produce cooling. Total opening area and opening size and position show a significant effect on pressure drop, air distribution uniformity and cooling efficiency. Recent advances in measurement and mathematical modelling techniques have provided powerful tools to develop detailed investigations of local airflow rate and heat and mass transfer processes within complex packaging structures. The complexity of the physical structure of the packed systems and the biological variability of the produce make both experimental and model-based studies of transport processes challenging. In many of the available mathematical models, the packed structure is assumed as a porous medium; the limitations of the porous media approach are evident during vented package design studies principally when the containerto-produce dimension ratio is below a certain value. The complex and chaotic structure within horticultural produce ventilated packages during a forced-air precooling process complicates the numerical study of energy and mass transfer considering each individual produce. Future research efforts should be directed to detailed models of the vented package, the complex produce stacking within the package, as well as their interaction with adjacent produce, stacks and surrounding environment. For the validation of the numerical models, the development of better experimental techniques taking into account the complex packaging system is also very important

Nourishing the brain on deep space missions: nutritional psychiatry in promoting resilience

The grueling psychological demands of a journey into deep space coupled with ever-increasing distances away from home pose a unique problem: how can we best take advantage of the benefits of fresh foods in a place that has none? Here, we consider the biggest challenges associated with our current spaceflight food system, highlight the importance of supporting optimal brain health on missions into deep space, and discuss evidence about food components that impact brain health. We propose a future food system that leverages the gut microbiota that can be individually tailored to best support the brain and mental health of crews on deep space long-duration missions. Working toward this goal, we will also be making investments in sustainable means to nourish the crew that remains here on spaceship Earth