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1.
A newly developed mini-scale high shear granulator was used for scale-up study of wet granulation process from 0.2 to 200 L scales. Under various operation conditions and granulation bowl sizes, powder mixture composed of anhydrous caffeine, D-mannitol, dibasic calcium phosphate, pregelatinized starch and corn starch was granulated by adding water. The granules were tabletted, and disintegration time and hardness of the tablets were evaluated to seek correlations of granulation conditions and tablet properties. As the granulation proceeded, disintegration time was prolonged and hardness decreased. When granulation processes were operated under the condition that agitator tip speed was the same, similar relationship between granulation time and tablet properties, such as disintegration time and hardness, between 0.2 L and 11 L scales were observed. Likewise, between 11 L and 200 L scales similar relationship was observed when operated under the condition that the force to the granulation mass was the same. From the above results, the mini-scale high shear granulator should be useful tool to predict operation conditions of large-scale granulation from its mini-scale operation conditions, where similar tablet properties should be obtained.  相似文献   

2.
Abstract

This preliminary study has mainly focused on the wax identification by nuclear magnetic resonance (NMR) and removal. Wax is used for many purposes in the field of art as protective coatings on wooden, stone or metal objects. From the comparison of the spectra H NMR and in particular with the correspondence of the resonance peaks of the samples taken from the statue and beeswax and paraffin, we can conclude that the wax applied on the statue surface is beeswax. From our data, it can be concluded that, to remove the beeswax, from any stone support, the more effective solvent is the mixture of cyclohexane/ethyl acetate. The removal percentages ranged from 19 to 99%. Lower percentages of removal have been observed in the case of yellow marble, probably because of its high porosity. We can affirm that, this solvent mixture can be employed in real art objects using cotton swabs to remove protective wax.  相似文献   

3.
The objective of this study was to characterize the properties of pectin extracted from sugar beet pulp using subcritical water (SWE) as compared to conventional extraction (CE). The research involved advanced modeling using response surface methodology and optimization of operational parameters. The optimal conditions for maximum yield of pectin for SWE and CE methods were determined by the central composite design. The optimum conditions of CE were the temperature of 90 °C, time of 240 min, pH of 1, and pectin recovery yield of 20.8%. The optimal SWE conditions were liquid-to-solid (L/S) ratio of 30% (v/w) at temperature of 130 °C for 20 min, which resulted in a comparable yield of 20.7%. The effect of obtained pectins on viscoamylograph pasting and DSC thermal parameters of corn starch was evaluated. The contents of galacturonic acid, degree of methylation, acetylation, and ferulic acid content were higher in the pectin extracted by SWE, while the molecular weight was lower. Similar chemical groups were characterized by FTIR in both SWE and CE pectins. Color attributes of both pectins were similar. Solutions of pectins at lower concentrations displayed nearly Newtonian behavior. The addition of both pectins to corn starch decreased pasting and DSC gelatinization parameters, but increased ΔH. The results offered a promising scalable approach to convert the beet waste to pectin as a value-added product using SWE with improved pectin properties.  相似文献   

4.
The objective of the present study is to enhance the resistant starch (RS) content of high amylose rice starch with heat–moisture treatment (HMT) for industrial application. The optimized HMT condition for achieving the highest RS content established using response surface methodology (RSM) was a temperature of 100 °C, moisture content of 24.2%, and a time of 11.5 h. Upon HMT, the RS content increased from 32.1% for native starch to 46.4% in HMT starch with optimized condition. HMT of the starches reduced the solubility and swelling power. The surface of HMT starch granules was more irregular than native starch. The X-ray diffraction (XRD) peak intensity at 2θ = 5° was greatly reduced by HMT, and the peaks at 22.7° and 24.2° were merged. HMT increased the gelatinization temperature and reduced the gelatinization enthalpy. HMT provides a method for the production of high-yield RS2 with high amylose rice starch in industrial application.  相似文献   

5.
A European interlaboratory study was conducted to validate an analytical procedure for the detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate. In principle, the fat obtained from plain chocolate according to the Soxhlet principle is separated by high-resolution capillary gas chromatography into triacylglycerol fractions according to their acyl-C-numbers, and within a given number, also according to unsaturation. The presence of cocoa butter equivalents is detected by linear regression analysis applied to the relative proportions of the 3 main triacylglycerol fractions of the fat analyzed. The amount of the cocoa butter equivalent admixture is estimated by partial least-squares regression analysis applied to the relative proportions of the 5 main triacylglycerols. Cocoa butter equivalent admixtures were detected down to a level of 2% related to the fat phase, corresponding to 0.6% in chocolate (assumed fat content of chocolate, 30%), without false-positive or -negative results. By using a quantification model based on partial least-squares regression analysis, the predicted cocoa butter equivalent amounts were in close agreement with the actual values. The applied model performed well at the level of the statutory limit of 5% cocoa butter equivalent addition to chocolate with a prediction error of 0.6%, assuming a chocolate fat content of 30%.  相似文献   

6.
The content of polyphenols in chocolate depends on many factors related to the properties of raw material and manufacturing parameters. The trend toward developing chocolates made from unroasted cocoa beans encourages research in this area. In addition, modern customers attach great importance to how the food they consume benefits their bodies. One such benefit that consumers value is the preservation of natural antioxidant compounds in food products (e.g., polyphenols). Therefore, in our study we attempted to determine the relationship between variable parameters at the conching stage (i.e., temperature and time of) and the content of dominant polyphenols (i.e.,catechins, epicatechins, and procyanidin B2) in chocolate milk mass (CMM) obtained from unroasted cocoa beans. Increasing the conching temperature from 50 to 60 °C decreased the content of three basic flavan-3-ols. The highest number of these compounds was determined when the process was carried out at 50 °C. However, the time that caused the least degradation of these compounds differed. For catechin, it was 2 h; for epicatechin it was 1 h; and for procyanidin it was 3 h. The influence of both the temperature and conching time on the rheological properties of chocolate milk mass was demonstrated. At 50 °C, the viscosity and the yield stress of the conched mass showed its highest value.  相似文献   

7.
The development and in-house testing of a method for the detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate is described. A database consisting of the triacylglycerol profile of 74 genuine cocoa butter and 75 cocoa butter equivalent samples obtained by high-resolution capillary gas liquid chromatography was created, using a certified cocoa butter reference material (IRMM-801) for calibration purposes. Based on these data, a large number of cocoa butter/cocoa butter equivalent mixtures were arithmetically simulated. By subjecting the data set to various statistical tools, reliable models for both detection (univariate regression model) and quantification (multivariate model) were elaborated. Validation data sets consisting of a large number of samples (n = 4050 for detection, n = 1050 for quantification) were used to test the models. Excluding pure illipé fat samples from the data set, the detection limit was determined between 1 and 3% foreign fat in cocoa butter. Recalculated for a chocolate with a fat content of 30%, these figures are equal to 0.3-0.9% cocoa butter equivalent. For quantification, the average error for prediction was estimated to be 1.1% cocoa butter equivalent in cocoa butter, without prior knowledge of the materials used in the blend corresponding to 0.3% in chocolate (fat content 30%). The advantage of the approach is that by using IRMM-801 for calibration, the established mathematical decision rules can be transferred to every testing laboratory.  相似文献   

8.
The indiscriminate use of plastic in food packaging contributes significantly to environmental pollution, promoting the search for more eco-friendly alternatives for the food industry. This work studied five formulations (T1–T5) of biodegradable cassava starch/gelatin films. The results showed the presence of the starch/gelatin functional groups by FT-IR spectroscopy. Differential scanning calorimetry (DSC) showed a thermal reinforcement after increasing the amount of gelatin in the formulations, which increased the crystallization temperature (Tc) from 190 °C for the starch-only film (T1) to 206 °C for the film with 50/50 starch/gelatin (T3). It also exhibited a homogeneous surface morphology, as evidenced by scanning electron microscopy (SEM). However, an excess of gelatin showed low compatibility with starch in the 25/75 starch/gelatin film (T4), evidenced by the low Tc definition and very rough and fractured surface morphology. Increasing gelatin ratio also significantly increased the strain (from 2.9 ± 0.5% for T1 to 285.1 ± 10.0% for T5) while decreasing the tensile strength (from 14.6 ± 0.5 MPa for T1 to 1.5 ± 0.3 MPa for T5). Water vapor permeability (WVP) increased, and water solubility (WS) also decreased with gelatin mass rising in the composites. On the other hand, opacity did not vary significantly due to the films’ cassava starch and gelatin ratio. Finally, optimizing the mechanical and water barrier properties resulted in a mass ratio of 53/47 cassava starch/gelatin as the most appropriate for their application in food packaging, indicating their usefulness in the food-packaging industry.  相似文献   

9.
The aim of this study was to estimate the contamination of grain coffee, roasted coffee, instant coffee, and cocoa purchased in local markets with ochratoxin A (OTA) and its isomerization product 2′R-ochratoxin A (2′R-OTA), and to assess risk of dietary exposure to the mycotoxins. OTA and 2′R-OTA content was determined using the HPLC chromatography with immunoaffinity columns dedicated to OTA. OTA levels found in all the tested samples were below the maximum limits specified in the European Commission Regulation EC 1881/2006. Average OTA concentrations calculated for positive samples of grain coffee/roasted coffee/instant coffee/cocoa were 0.94/0.79/3.00/0.95 µg/kg, with the concentration ranges: 0.57–1.97/0.44–2.29/0.40–5.15/0.48–1.97 µg/kg, respectively. Average 2′R-OTA concentrations calculated for positive samples of roasted coffee/instant coffee were 0.90/1.48 µg/kg, with concentration ranges: 0.40–1.26/1.00–2.12 µg/kg, respectively. In turn, diastereomer was not found in any of the tested cocoa samples. Daily intake of both mycotoxins with coffee/cocoa would be below the TDI value even if the consumed coffee/cocoa were contaminated with OTA/2′R-OTA at the highest levels found in this study. Up to now only a few papers on both OTA and 2′R-OTA in roasted food products are available in the literature, and this is the first study in Poland.  相似文献   

10.
This paper reports the precise analysis of the eutectic mixing behavior of 1,3-distearoyl-2-oleoyl-sn-glycerol (SOS) and trilaurin (LLL), as a typical model case of the mixture of cocoa butter (CB) and cocoa butter substitute (CBS). SOS was mixed with LLL at several mass fractions of LLL (wLLL); the mixtures obtained were analyzed for polymorphic phase behavior using differential scanning calorimetry (DSC) and synchrotron radiation X-ray diffractometry (SR-XRD). In melt crystallization with constant-rate cooling, SOS and LLL formed eutectics in their metastable polymorphs, allowing the occurrence of a compatible solid solution at wLLL ≥ 0.925. With subsequent heating, the resultant crystals transformed toward more stable polymorphs, then melted in a eutectic manner. For mixtures aged at 25 °C after melt crystallization, eutectics were found in the extended wLLL region, even at wLLL = 0.975. These results indicate that phase separation between SOS and LLL progressed in their solid solution under stabilization. The crystal growth of the separated SOS fraction may cause fat-bloom formation in compound chocolate containing CB and CBS. To solve this problem, the development of retardation techniques against phase separation is expected.  相似文献   

11.
The aim of this study was to evaluate the levels of chemical markers in raw cacao beans in two clones (introduced and regional) in Colombia over several years. Multivariate statistical methods were used to analyze the flavanol monomers (epicatechin and catechin), flavanol oligomers (procyanidins) and methylxanthine alkaloids (caffeine and theobromine) of cocoa samples. The results identified genotype as the main factor contributing to cacao chemistry, although significant differences were not observed between universal and regional clones in PCA. The univariate analysis allowed us to establish that EET-96 had the highest contents of both flavanol monomers (13.12 ± 2.30 mg/g) and procyanidins (7.56 ± 4.59 mg/g). In addition, the geographic origin, the harvest conditions of each region and the year of harvest may contribute to major discrepancies between results. Turbo cocoa samples are notable for their higher flavanol monomer content, Chigorodó cocoa samples for the presence of both types of polyphenol (monomer and procyanidin contents) and the Northeast cocoa samples for the higher methylxanthine content. We hope that knowledge of the heterogeneity of the metabolites of interest in each clone will contribute to the generation of added value in the cocoa production chain and its sustainability.  相似文献   

12.
The formulation of Garcinia kola seeds into tablet dosage form and evaluation of some physical properties of the tablets are presented. A chemical assay was conducted on the dry, powdered seeds as well as the crude aqueous extract of the seeds. The dry powdered seeds contain 0.003% of flavonoids while the crude extract contained 0.007% of flavonoids based on rutin used as the standard. The powdered material (50 mg) and crude extract (10 mg) were formulated into tablets using the wet granulation method. Named binders were evaluated in these formulations. The various tablet parameters were evaluated, namely: weight variation, thickness and diameter, hardness, friability, disintegration time, dissolution profile and content uniformity. The results indicated that the tablets had good disintegration time, dissolution and hardness/friability profiles. Tablets formulated with starch had the best disintegration properties but were consequently very friable. Tablets formulated from 10 mg of the crude extract needed a larger proportion of diluents, which affected the tablet properties.  相似文献   

13.
Summary Analysis of the IR spectra of waxes isolated from samples of paints from paintings dating from the Ist to VIIth centuries of our era and fragments of archaeological antique murals has shown that in some cases the wax isolated is pure beeswax and in others it contains as impurities what are presumably resin acids, and also salts of fatty acids. The IR spectrum of pure beeswax extracted from a fragment buried for 2000 yr is absolutely identical with the spectrum of modern beeswax, which shows the extreme chemical stability of the wax.All-Union Central Scientific-Research Laboratory for Conservation and Restoration, Moscow. Scientific-Research Institute of Organic Intermediates and Dyes, Moscow. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 271–275, March–April, 1977.  相似文献   

14.
Petroleum, synthetic, and natural waxes have been used as hydrophobic bases for dispersions intended for use as barrier coatings for packaging paper. Oil-in-water dispersions with alkaline pH were prepared by a two-step homogenization procedure containing paraffin wax, with various characteristics, the Fischer–Tropsch synthesis product or beeswax. The size of the dispersed particles determined by dynamic light scattering depended on the type of hydrophobic base used and was in the range of 350–440 nm. The ability of dispersion particles in aggregation driven by electrostatic attraction, evaluated by Zeta potential analysis by electrophoretic light scattering, was from −26 to −50 mV. Static multiply light scattering was used for 30 days of stability assessment and helped to select the dispersion with a Sarawax SX70 wax base as the most stable. Dispersions were further used for coating the backing of kraft paper by the Meyer rod method. Coated paper with an applied coating of 6 g/m2 had very good hydrophobic properties (Cobb60 < 4 g/m2), sufficient strength properties, and air permeation, which enabled its application as a packaging material. The dispersions based on Sarawax SX70 wax were evaluated as the best coating for Mondi ProVantage Kraftliner 125 g/m2 backing paper. Good hydrophobic properties and strength properties indicate the possibility of using the SX70-based wax dispersion coating as a replacement for PFAS coatings in some applications.  相似文献   

15.
This study aimed to obtain a third-generation snack from native rice starch (NS), rice starch modified by extrusion (MS), nopal flour (NF) and xanthan gum (XG). These raw materials were characterized by proximal analysis, pH, particle size distribution, water absorption index (WAI) and water solubility index (WSI), degree of substitution (DS), differential scanning calorimetry (DSC), rheology, Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The analysis of the response variables in the nine formulations of the snack: expansion index (EI), apparent density (AD), hardness (H), luminosity (L*) and tendency to green-red (a*), was performed through a composite central design (CCD), the selected formulations were characterized by SEM. Results showed an increase in WAI, 4.69 ± 0.04, and WSI, 12.61 ± 0.10, for MS, higher than NS values due to chemical modification. According to the color analysis the NF obtained a value of 60.73 ± 0.008 in L* and −6.51 ± 0.004 in a* with green tendency. The DS value obtained was 0.09 ± 0.005, being within the FDA’s permissible range for food use. By FTIR analysis, the acetyl group was corroborated. Finally, employing microwave cooking, snacks made from NS with concentrations of NF (5%) and XG (0%) obtained the highest EI value, 4.47, as well the low Dap and D value (0.37 g/cm3, 2.25 N, respectively), corroborated by SEM analysis.  相似文献   

16.
The objective of the current research is to develop ZnO-Manjistha extract (ZnO-MJE) nanoparticles (NPs) and to investigate their transdermal delivery as well as antimicrobial and antioxidant activity. The optimized formulation was further evaluated based on different parameters. The ZnO-MJE-NPs were prepared by mixing 10 mM ZnSO4·7H2O and 0.8% w/v NaOH in distilled water. To the above, a solution of 10 mL MJE (10 mg) in 50 mL of zinc sulfate was added. Box–Behnken design (Design-Expert software 12.0.1.0) was used for the optimization of ZnO-MJE-NP formulations. The ZnO-MJE-NPs were evaluated for their physicochemical characterization, in vitro release activity, ex vivo permeation across rat skin, antimicrobial activity using sterilized agar media, and antioxidant activity by the DPPH free radical method. The optimized ZnO-MJE-NP formulation (F13) showed a particle size of 257.1 ± 0.76 nm, PDI value of 0.289 ± 0.003, and entrapment efficiency of 79 ± 0.33%. Drug release kinetic models showed that the formulation followed the Korsmeyer–Peppas model with a drug release of 34.50 ± 2.56 at pH 7.4 in 24 h. In ex vivo studies ZnO-MJE-NPs-opt permeation was 63.26%. The antibacterial activity was found to be enhanced in ZnO-MJE-NPs-opt and antioxidant activity was found to be highest (93.14 ± 4.05%) at 100 µg/mL concentrations. The ZnO-MJE-NPs-opt formulation showed prolonged release of the MJE and intensified permeation. Moreover, the formulation was found to show significantly (p < 0.05) better antimicrobial and antioxidant activity as compared to conventional suspension formulations.  相似文献   

17.
超临界流体色谱流程设计及其应用   总被引:1,自引:1,他引:0  
周良模  沈玉峰 《分析化学》1993,21(8):983-987
本文设计了多功能超临界流体色谱流程,流程中包括毛细管/微填充柱SFC,GC,计算机控制温度、压力、密度及信号采集、处理,配置有超临界流体萃取池,解决了超临界流体色谱分流口易堵问题。利用该流程,将石腊、DC-200气相色谱固定相、黄油、蜂蜡、救心油、红花油等样品进行超临界流体色谱分离。  相似文献   

18.
Herein, we prepared 1,3-dipalmitoyl-2-oleoyl glycerol (POP)-rich fats with reduced levels of diacylglycerols (DAGs), adversely affecting the tempering of chocolate, via two-step hexane fractionation of palm stearin. DAG content in the as-prepared fats was lower than that in POP-rich fats obtained by previously reported conventional two-step acetone fractionation. Cocoa butter equivalents (CBEs) were fabricated by blending the as-prepared fats with 1,3-distearoyl-2-oleoyl glycerol (SOS)-rich fats obtained by hexane fractionation of degummed shea butter. POP-rich fats achieved under the best conditions for the fractionation of palm stearin had a significantly lower DAG content (1.6 w/w%) than that in the counterpart (4.6 w/w%) prepared by the previously reported method. The CBEs fabricated by blending the POP- and SOS-rich fats in a weight ratio of 40:60 contained 63.7 w/w% total symmetric monounsaturated triacylglycerols, including 22.0 w/w% POP, 8.6 w/w% palmitoyl-2-oleoyl-3-stearoyl-rac-glycerol, 33.1 w/w% SOS, and 1.3 w/w% DAGs, which was not substantially different from the DAG content in cocoa butter (1.1 w/w%). Based on the solid-fat content results, it was concluded that, when these CBEs were used for chocolate manufacture, they blended with cocoa butter at levels up to 40 w/w%, without distinctively altering the hardness and melting behavior of cocoa butter.  相似文献   

19.
A large quantity of longan fruits (Dimocarpus longan Lour.) produced annually are processed into many products, one of which is black longan, from which the dried, dark-brown meat has been used medicinally in traditional medicine, while the starch-containing seeds are discarded. In this study, starch samples (BLGSs) were isolated from seeds of black longan fruits prepared using varied conditions. The in vitro digestibility was determined in comparison with those extracted from fresh (FLGS) and dried (DLGS) seeds. Scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy were employed to evaluate the starch properties. The results showed that the yields of FLGS, DLGS, and BLGSs were 20%, 23%, and 16–22% w/w, respectively. SEM images showed starch granules of mixed shapes, with sizes up to 15 µm in all samples. XRD patterns confirmed an A-type crystallinity for FLGS and DLGS, with strong refraction peaks at 2θ = 15°, 17°, 18°, and 23°, while BLGSs also showed detectable peaks at 2θ = 10° and 21°, which suggested V-type structures. Thermal properties corroborated the changes by showing increases in peak gelatinization temperature (Tp) and enthalpy energy (ΔH) in BLGSs. The paste viscosity of BLGSs (5% w/w) decreased by 20–58% from that of FLGS. The FTIR peak ratio at 1045/1022 and 1022/995 cm−1 also indicated an increase in ordered structure in BLGSs compared to FLGS. The significant increase in the amounts of slowly digestible starch (SDS) and resistant starch (RS) in BLGSs compared to FLGS, especially at a prolonged incubation time of 20 (4.2×) and 30 days (4.1×), was proposed to be due to the heat-induced formation of starch inclusion with other components inside the seed during the black longan production process. Thus, black longan seed could be a new source of starch, with increased RS content, for potential use in the food and related industries.  相似文献   

20.
Essential oils (EOs) are naturally occurring volatile aromatic compounds extracted from different parts of plants. They are made up of components like terpenes, phenols, etc., and are chemically unstable and susceptible to oxidative deterioration, leading to reduced shelf-life and overall degradation of the product. Encapsulation of EOs in a matrix can prevent degradation of the active ingredient and improve the shelf-life. In this paper, we report encapsulation of Dhavana oil (Artemisia pellen) in a modified starch matrix using a spray-drying technique. Physico-chemical properties of neat and encapsulated Dhavana oil were studied. We selected two powder bases: CaCO3 and TALC and, loaded neat and encapsulated Dhavana oil in it, studied their stability and interaction with the base matrices at 3 °C, 22 °C and 45 °C up to 2 months under closed conditions and one week at 22 °C and 45 °C under open condition. Thermal degradation pattern was studied for neat and encapsulated Dhavana oil and modified starch. Release of primary active component of neat and encapsulated Dhavana oil from the base matrices was evaluated with GCMS. Stability study and release mechanism were elucidated to understand the release pattern in different base powders under similar conditions. Retention of hydroxydhavanone was found to be better in TALC than CaCO3, and therefore, the former can be considered a suitable base matrix for developing a stable powder formulation with an optimum release of the oil. Dhavana oil is known for its anti-microbial activity, and hence, neat and encapsulated Dhavana oil was tested on different bacterial and fungal strains. The encapsulated oil depicted good anti-microbial efficacy against various bacterial and fungal strains, which is a step forward for developing anti-microbial formulations. Thus, the reported work will provide helpful information on cosmetic formulation and, therefore, be useful for perfumery, food, and cosmetic industries.  相似文献   

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