Effect of cryogenic grinding on volatile and fatty oil constituents of cumin (Cuminum cyminum L.) genotypes.

Effect of cryogenic grinding on recovery of volatile oil, fatty oil percentage and their constituents in two cumin (Cuminum cyminum L.) genotypes have been analyzed. Cryogenic grinding not only retains the volatiles but enhanced the recovery by 33.9 % in GC 4 and 43.5 % in RZ 209. A significant increase (29.9 %) over normal grinding in oil percentage was also observed in genotype RZ 209. This increase was, however, less (15.4 %) in genotype GC 4. Nineteen major compounds were identified in the essential oil of both genotypes. The two grinding techniques had significant effects on dependent variables, viz., volatile oil and monoterpenes. Cuminaldehyde was the main constituent in both genotypes, content of which increased from 48.2 to 56.1 % in GC 4 on cryo grinding. Content of terpines were found to decrease in cryo ground samples of GC 4 and either decrease or no change was found in RZ 209. Organoleptic test showed more pleasant aroma in cryo ground seeds of both the genotypes. Significant increase was also reported in fatty oil yield due to cryogenic grinding. Fatty acid methyl ester (FAME) analysis showed oleic acid as major FAME content of which increased from 88.1 to 94.9 % in RZ 209 and from 88.2 to 90.1 % in GC 4 on cryogenic grinding. Other prominent FAME were palmitic, palmitoleic and stearic acid. Results indicated commercial potential of cryogenic grinding technology for cumin in general and spices in particular for better retention of flavour and quality in spices.

A Production and Fractionation Protocol for Polyvinyl Chloride Microplastics.

Concerns about the presence of microplastics in the environment has increased in recent years, prompting more attention from scientists. Thorough exposure studies using artificially produced microplastics containing additives are required to assess their potentially hazardous effects. Therefore, an efficient microplastic production and fractionation protocol was established using a cryogenic grinding and wet-sieving approach. The developed cryogenic grinding method was able to produce (20-40 g/h) polyvinyl chloride (PVC) microplastics having a volume-weighted mean particle size of 391 µm and a span of 2.12. Performing a second grinding cycle on the same particles resulted in microplastics which were smaller (volume-weighted mean size = 219 µm) and had a narrower particle size distribution (span = 1.59). In addition, the microplastics were also fractionated into different particle size ranges using a vibrating wet-sieving tower. The latter technique allowed separating 10 g of PVC microplastics into seven different fractions using six sieves (Ø 200 mm) for 30 min while shaking. By using the developed method, PVC microplastics could easily be made and fractionated into desired particle-size ranges. The proposed protocol could also be adjusted to produce and fractionate microplastics of other plastics.

Nanofiber Fractionalization Stimulates Healing of Large Intestine Anastomoses in Rabbits.

Background: A current topic of ma jor interest in regenerative medicine is the development of novel materials for accelerated healing of sutures, and nanofibers seem to be suitable materials for this purpose. As various studies have shown, nanofibers are able to partially substitute missing extracellular matrix and to stimulate cell proliferation and differentiation in sutures. Therefore, we tested nanofibrous membranes and cryogenically fractionalized nanofibers as potential materials for support of the healing of intestinal anastomoses in a rabbit model. Materials and Methods: We compared cryogenically fractionalized chitosan and PVA nanofibers with chitosan and PVA nanofiber membranes designed for intestine anastomosis healing in a rabbit animal model. The anastomoses were biomechanically and histologically tested. Results: In strong contrast to nanofibrous membranes, the fractionalized nanofibers did show positive effects on the healing of intestinal anastomoses in rabbits. The fractionalized nanofibers were able to reach deep layers that are key to increased mechanical strength of the intestine. Moreover, fractionalized nanofibers led to the formation of collagen-rich 3D tissue significantly exceeding the healing effects of the 2D flat nanofiber membranes. In addition, the fractionalized chitosan nanofibers eliminated peritonitis, significantly stimulated anastomosis healing and led to a higher density of microvessels, in addition to a larger fraction of myofibroblasts and collagen type I and III. Biomechanical tests supported these histological findings. Conclusion: We concluded that the fractionalized chitosan nanofibers led to accelerated healing for rabbit colorectal anastomoses by the targeted stimulation of collagen-producing cells in the intestine, the smooth muscle cells and the fibroblasts. We believe that the collagen-producing cells were stimulated both directly due to the presence of a biocompatible scaffold providing cell adhesion, and indirectly, by a proper stimulation of immunocytes in the suture.

Encapsulation of Lactobacillus acidophilus in solid lipid microparticles via cryomilling.

We herein delved into the microencapsulation of Lactobacillus acidophilus (LA) into solid lipid microparticles (SLMs) via the cryomilling technique. For this aim, a frozen lipid mixture containing LA was pulverized at different times (7, 14, 21, 28, and 35 min) using a cryogenic mixer mill to produce probiotic-loaded SLMs. The impacts of different cryomilling durations on the SLMs properties (morphology, particle size, water activity, polymorphism, crystallinity, and thermal behavior) and the viability of LA were evaluated. Microencapsulation improved the viability of LA in simulated gastrointestinal fluids, heat stress, and different concentrations of salt and sucrose. SLMs also were suitable to be incorporated into foods. However, once the cryomilling time was prolonged, the viability of encapsulated LA declined, and particle size grew. The cryomilling technique showed great potential as an alternative approach for encapsulation due to the lack of solvent, short processing time, and simplicity.

Trends in Grinding of Agroindustrial Products-A Literature Review.

BACKGROUND: This article aims to present the results of a literature review on food milling, to identify the most recent uses, types of mills, and new grinding trends. METHODS: For this, a search was made with the keywords "grinding", "milling" and "food" in the Scopus, which yielded 192 articles, 52 of which directly related to food, were analyzed. RESULTS: Contributions were found related to various types of grinding such as cryogenic grinding, nano-scaled grinding, ultrafine and superfine grinding. The authors highlighted the uses of these types of milling in agro-industrial products such as nutmeg (Myristica fragrans), wheat bran (Triticum spp.), ginger (Zingiber officinale), and green tea powder (Camellia sinensis), among others. CONCLUSION: It is observed that engineering texts dealing with theoretical and analytical food milling operations do not emphasize the new trends found. As a complementary part of this study, eight patents related to cryogenic grinding in food were analyzed, identifying uses of this type of grinding in coffee, lipids, lycopene, proteins, grains, and seeds. Besides, a search was carried out to find out commercial suppliers of cryogenic grinding equipment, in which six companies from China with their equipment were identified.

Effect of Cryogenic Grinding on Fatigue Life of Additively Manufactured Maraging Steel.

Additive manufacturing (AM) is replacing conventional manufacturing techniques due to its ability to manufacture complex structures with near-net shape and reduced material wastage. However, the poor surface integrity of the AM parts deteriorates the service life of the components. The AM parts should be subjected to post-processing treatment for improving surface integrity and fatigue life. In this research, maraging steel is printed using direct metal laser sintering (DMLS) process and the influence of grinding on the fatigue life of this additively manufactured material was investigated. For this purpose, the grinding experiments were performed under two different grinding environments such as dry and cryogenic conditions using a cubic boron nitride (CBN) grinding wheel. The results revealed that surface roughness could be reduced by about 87% under cryogenic condition over dry grinding. The fatigue tests carried out on the additive manufactured materials exposed a substantial increase of about 170% in their fatigue life when subjected to cryogenic grinding.

Balancing sugar recovery and inhibitor generation during energycane processing: Coupling cryogenic grinding with hydrothermal pretreatment at low temperatures.

Pretreatment of lignocellulosic biomass at high temperatures or with oxidizing chemicals generate various inhibitors that restrict the efficient bioconversion of sugars in subsequent steps. The present study systematically investigates individual and combinatorial effects of pretreatment parameters on the generation of inhibitors. A plot between pretreatment temperature and inhibitor revealed optimum pretreatment temperature for energycane bagasse i.e., 170 °C beyond which total inhibitor production increased exponentially. No inhibitor production was observed on mechanical processing i.e., disk milling/cryogenic grinding of biomass. Evaluation of response surface regression exhibited that biomass solids loading has a significant effect on inhibitor generation at higher temperatures. The concentrations of certain inhibitors such as acetic acid, furfurals, and HMF increased more than 3-folds on doubling the solids loading. Furthermore, a novel low-severity approach of low-temperature hydrothermal pretreatment coupled with cryogenic grinding for lignocellulosic biomasses has been introduced which improved sugar yields while maintaining a low inhibitor concentration.

Roasting and Cryogenic Grinding Enhance the Antioxidant Property of Sword Beans (Canavalia gladiata).

The objective of this study was to optimize the conditions for enhancing the antioxidant properties of sword bean (Canavalia gladiata) as a coffee substitute in two processing methods, roasting and grinding. The optimum conditions for removing off-flavor of the bean and maximizing functionality and efficiency were light roasting and cryogenic grinding (< 53 µm). In these conditions, extraction yield was 16.75%, total phenolic content (TPC) was 69.82 ± 0.35 mg gallic acid equivalents/g, and total flavonoid content (TFC) was 168.81 ± 1.64 mg quercetin equivalents/100 g. The antioxidant properties were 77.58 ± 0.27% for DPPH radical scavenging activity and 58.02 ± 0.76 mg Trolox equivalents/g for ABTS radical scavenging activity. The values for TFC and ABTS radical scavenging activity were significantly higher (p < 0.05) than in other conditions, and TPC and DPPH radical scavenging activity were second highest in lightly roasted beans, following raw beans. HS-SPME/GCMS analysis confirmed that the amino acids and carbohydrates, which are the main components of sword bean, were condensed into other volatile flavor compounds, such as derivatives of furan, pyrazine, and pyrrole during roasting. Roasted and cryogenically ground (cryo-ground) sword beans showed higher functionality in terms of TFC, DPPH, and ABTS radical scavenging activities compared to those of coffee. Overall results showed that light roasting and cryogenic grinding are the most suitable processing conditions for enhancing the bioactivity of sword beans.

Comparison of volatile compounds in different parts of fresh Amomum villosum Lour. from different geographical areas using cryogenic grinding combined HS-SPME-GC-MS.

BACKGROUND: The essential oil is one of the main active ingredients of Amomum villosum Lour. However, volatile compounds are easily lost during the drying, storage and even sample preparation procedure. Therefore, using fresh samples can obtain more accurately data for qualitative and comparative analysis. METHODS: In this study, the volatile compounds in different parts of fresh A. villosum from different origins were systemic analyzed and compared by using cryogenic grinding combined HS-SPME-GC-MS for the first time. GC-MS analyses were performed on a 6890 Series GC instrument coupled to a 5973 N mass spectrometer. The volatile compounds were extracted by the SPME fiber (100 µm PDMS). Analytes separation was achieved on a HP-5MS capillary column. The oven temperature was initially programmed at 70 °C, then raised 4 °C/min to reach 125 °C and then programmed at 0.5 °C/min to 133 °C, then at 6 °C/min to 170 °C and finally, at 20 °C/min to 280 °C held for 2 min. The temperatures of the injection port, ion source and transfer line were set at 250 °C, 230 °C and 280 °C, respectively. RESULTS: Forty-eight main compounds were identified in different parts of fresh A. villosum. The most abundant components in fresh fruit samples were camphor (3.91%), bornyl acetate (10.53%), caryophyllene (8.70%), ß-bisabolene (11.50%), (E)-nerolidol (14.82%) and cubenol (10.04%). This is quite different with that of dried samples analyzed in our previous work. As different parts of the same plant, many common components with biological activities were detected in fruit and other parts. In principle components analysis (PCA) and hierarchical clustering analysis (HCA), four parts of A. villosum were divided into different groups clearly. Additionally, fruit and root samples also could be divided into two subgroups (HCA) in accordance with their regions. CONCLUSION: The developed method was successfully used for qualitative and comparative analysis of volatile compounds in fresh A. villosum samples. Additionally, using fresh samples can obtain much more information which is helpful for their performance in the fields of functional foods, agriculture and biomedical industry. Furthermore, our research is helpful for comprehensive utilization and quality control of A. villosum.

Separation of the cathode materials from the Al foil in spent lithium-ion batteries by cryogenic grinding.

An environmentally friendly technology of cryogenic grinding for recovering cathode materials from spent lithium-ion batteries was has been investigated in this paper. Differential Scanning Calorimeter was used to test the glass transition temperature of the organic binder. Advanced analysis techniques, a microcomputer-controlled electronic universal material-testing machine, a low-temperature impact testing machine, scanning electron microscopy and high-resolution 3 Dimension-X-ray microscopy, were utilized to analyze the effect of low temperature on the mechanical properties and morphology of cathode. Results show that the yield strength, tensile strength and impact strength of the current collector is significantly increased at low temperature, that the glass transition temperature of the organic binder is approximately 235 K. Low temperature enhances the strength of the current collector and causes the organic binder to fail. Therefore, cryogenic grinding could realize the selective grinding of the cathode and significantly improve the peel-off of the electrode materials. The peel-off efficiency of cathode materials was improved from 25.03% to 87.29% at the optimum conditions of low temperature pretreatment for 5 min and cryogenic grinding for 30 s. The experiments demonstrate that the cryogenic grinding can obviously facilitate the efficient recovery of cathode materials, revealing a great application prospective for the recycling of spent lithium-ion batteries.

The cryogenic grinding as the important homogenization step in analysis of inconsistent food samples.

Some homogenisation approaches have been investigated to make easier and overcome troublesome preparation of inconsistent food samples. Contents of Na, Ca, Mg, P, Fe, Mn and Zn in muesli, seed and instant food samples were determined by inductively coupled plasma optical emission spectrometry after their grinding with an agate mortar, a kitchen coffee grinder and a cryogenic mill. The efficiency of a grinding step was evaluated using RSDs and homogeneity factors (H-factor). For cryogenically grinded samples, RSDs were detected about 4% and H-factors on 10, what is acceptable for the analytical purpose. The results for grinding with an agate mortar as well as a coffee grinder were quite unsatisfactory (RSDs in tens percent). Differences between RSDs and H-factors for the procedures tested were detected to be statistically significant. Different element contents were observed in differently treated samples which is probably a result of an unevenly element distribution in inhomogeneous components forming sample.

Liberation characteristics after cryogenic modification and air table separation of discarded printed circuit boards.

Liberating useful materials from printed circuit boards (PCBs) is challenging because PCBs are flexible and complex in terms of materials and components. In this study, the crushing of PCBs at low-temperature was investigated. The results indicated that when the temperature was decreased to approximately -20 °C, the strength of PCBs decreased and their brittleness increased, making them easier to crush. A double roll crusher was selected to crush the PCBs. The particle size distribution and power consumption were studied under different working conditions. The results showed that the particle size of most of the lumps was in the range 15×20-25×20 mm, and that power consumption was minimal when the frequency of the crusher was 40-50 Hz. A small shredder was used for cryogenic grinding, and it was found that its power consumption strongly depended on the cooling temperature. An orthogonal experiment was conducted, which revealed that a smaller cutter gap and higher rotational speed could achieve higher yield. Furthermore, the results indicated that the air table developed to liberate PCB materials could effectively separate 2.8-0.5mm grade materials. Overall, the results of this study provide an experimental foundation for more effectively recycling discarded PCBs.

Mechanistic insight into the dramatic improvement of probucol dissolution in neutral solutions by solid dispersion in Eudragit E PO with saccharin.

OBJECTIVES: Solid dispersion using Eudragit E PO (EPO) improves the dissolution of poorly water-soluble drugs in acidic solutions; however, the dissolution extremely decreases in neutral solutions. In this report, ternary solid dispersions containing probucol (PBC), EPO, and saccharin (SAC) were prepared to enable high drug dissolution at neutral pH. METHODS: Cryogenic-grinding was used to obtain ternary solid dispersions. Dissolution tests at neutral pH values were conducted to confirm the usefulness of the cryogenic-ground mixture (cryo-GM). The molecular state of each component and intermolecular interactions in the ternary cryo-GM were evaluated using powder X-ray diffraction (PXRD) and (13) C solid-state NMR including spin-lattice relaxation time evaluation. KEY FINDINGS: PBC dispersed in ternary cryo-GM had an improved dissolution in neutral solutions. PBC and SAC were in amorphous states in EPO polymer matrices. The weak hydrophobic interaction between PBC and EPO and the ionic bond or hydrogen bond between EPO and SAC were demonstrated. These two molecular interactions improved the dissolution of PBC in neutral solutions. CONCLUSION: Preparation of ternary solid dispersion is a potential method of improving drug solubility and absorption.

The effect of cryogenic grinding and hammer milling on the flavour quality of ground pepper (Piper nigrum L.).

In this study, we compared the effects of cryogenic grinding and hammer milling on the flavour attributes of black, white, and green pepper. The flavour attributes were analysed using headspace solid-phase micro-extraction (HS-SPME) and gas chromatography-mass spectrometry (GC/MS), sensory evaluation and electronic nose (e-nose) analysis. Cryogenic grinding resulted in minimal damage to the colour, flavour, and sensory attributes of the spices. Cryogenic grinding was also better than hammer milling at preserving the main potent aroma constituents, but the concentrations of the main aroma constituents were dramatically reduced after storing the samples at 4 °C for 6 months. Pattern matching performed by the e-nose further supported our sensory and instrumental findings. Overall, cryogenic grinding was superior to hammer milling for preserving the sensory properties and flavour attributes of pepper without significantly affecting its quality. However, we found that the flavour quality of ground pepper was reduced during storage.