Preparation and characterization of nanoparticles based on hydrophobic alginate derivative as carriers for sustained release of vitamin D3

Hydrophobic alginate derivative was prepared by modification of alginate by acid chloride reaction using oleoyl chloride without organic solvents. The conjugate of oleoyl alginate ester (OAE) was confirmed by FT-IR and (1)H NMR. The degree of substitution (DS) of OAE was determined by (1)H NMR, and it ranged from 0.84 to 3.85. In distilled water, OAE formed self-assembled nanoparticles at low concentrations in aqueous medium, and nanoparticles retained their structural integrity both in simulated gastric fluid (SGF) and simulated intestinal fluid (SIF). The loading and release characteristics of nanoparticles based on OAE were investigated using vitamin D(3) as a model nutraceutical. As the concentration of vitamin D(3) increased, the loading capacity (LC) increased, whereas the loading efficiency (LE) decreased. Nanoparticles could release vitamin D(3) at a sustained rate in gastrointestinal fluid. These results revealed the potential of OAE nanoparticles as oral carriers for sustained release of vitamin D(3).     

Properties of zein films coated with drying oils

Zein films prepared by resin were coated with either flax oil or tung oil and cured by UV- or gamma-radiation. Coated zein films were then evaluated for tensile and water barrier properties. Film microstructure was examined by transmitted light microscope. Tensile strength, elongation, and toughness of oil-coated samples increased substantially with respect to uncoated films. Flax oil coated samples showed an increase in elongation of 300%. It was suggested that oil coatings fill in pinholes and cracks existing in zein films, affecting their mechanical properties. Water vapor permeability also decreased statistically for coated film (except for tung oil coated-UV treated films), suggesting water vapor transfer was controlled by film hydrophobicity and microstructure. Moreover, the liquid water transmission rate of coated films was at least 10 times slower than for control films. Examination of film microstructure revealed that flax oil coatings had uniform coverage and smooth finish, which explained their high elongation, low water vapor permeability. Tung oil coatings cured under UV light showed patterns of intertwined dark and light regions, which may be caused by cross-linking and drying at different times. The oriented structures were found when tung oil coatings were cured by gamma-radiation.     

包膜控释肥养分释放特性评价方法的研究进展

控释肥已成为国内外肥料研究的热点 ,但是评价控释肥养分释放特性的方法研究相对滞后 ,至今没有较为完善的方法和统一的测试标准。本文综述了包膜控释肥养分释放特性的现有评价方法 :水中 (或溶液 )溶出率法、土壤溶出率法、扩散率法、渗透率法、电超滤法和同位素示踪法等 ;评述了各种方法的优缺点及改进途径 ;并展望了今后评价方法的研究方向     

Alginate and chitosan functionalization for micronutrient encapsulation

A new method for encapsulation of micronutrients was successfully developed. The encapsulation matrix consisted of two polymers (alginate and chitosan), which were functionalized by acylation with palmitoyl chloride. The structural modifications of polymers were confirmed by Fourier transform infrared (FTIR) spectroscopy. Beads were formed by ionic gelation, and their mechanical and physical characteristics (puncture strength and deformation, viscoelasticity, water vapor permeability, and rate of gel swelling) were evaluated using beads or films made of bead-forming solutions. Functionalization increased elasticity and water impermeability of polymer films. Stability of selected encapsulated micronutrients (ferrous fumarate, ascorbic acid, and beta-carotene) was also evaluated under two levels of temperature (23 and 45 degrees C) and relative humidity (56 and 100%) for 6 months. Encapsulation strongly increased the stability of micronutrients. No difference was observed in the encapsulated micronutrients' stability between nonfunctionalized and functionalized beads. Finally, a release study in gastrointestinal media was conducted. Results showed that beads were not susceptible to enzymatic and acidic attacks during stomach transit. This research demonstrates the potential of a new encapsulation method to protect bioactive molecules from temperature, moisture, and acidic conditions.     

温度对壳聚糖包膜尿素氮素释放特性的影响

通过壳聚糖包膜尿素(CCU)在15℃、25℃、35℃、45℃水中的释放实验,描述了其养分释放特性,探讨了温度对CCU养分释放特性的影响。结果表明,壳聚糖包膜尿素与其他包膜尿素的释放情况有很大不同,不存在明显的滞后阶段。温度改变了包膜的通透性,CCU养分释放速率随着温度的增加而增大,温度每提高10℃,养分释放速率提高约1.5倍,但不同温度下养分累积释放曲线的变化具有相似性和规律性。在不同温度下,随着浸泡时间的延长,养分释放速率都是先线性降低,然后保持不变,直到尿素完全溶解,释放速率再次下降,直至为零。不同温度下CCU的水分透入率变化曲线与尿素累积释放量变化曲线相似,养分累积释放量和水分透入率呈线性关系。     

水溶性树脂包膜控释肥料养分释放特征及影响因素

为了探讨不同养分配比包膜控释肥料的养分释放特征,采用相同工艺制造同一包膜厚度而核心肥料氮磷钾配比（以下简称核心肥料）不同、同一核心肥料而包膜厚度不同的水溶性树脂包膜控释肥料,并在高温和常温下的纯水中培养,研究核心肥料、包膜厚度、培养温度对养分释放特征的影响。结果表明：在（25 ± 0.5）℃或（40 ± 0.5）℃下,膜材用量为50 g/m2和70 g/m2的高氮型控释肥料的养分累积释放特征曲线均呈S型,增加包膜厚度或降低培养温度,均可延长培养前期的养分缓慢释放阶段。在（25 ± 0.5）℃下,膜材用量为50 g/m2时,均衡型和高钾型控释肥料的养分累积释放曲线为抛物线型,膜材用量为70 g/m2时,则为双抛物线型;培养温度为（40 ± 0.5）℃时,养分累积释放曲线均转变为抛物线型。3种因素不仅影响养分释放曲线的形状,同时对肥效期产生明显影响,增加包膜厚度或降低培养温度,均可延长养分的肥效期。氮磷的肥效期大小顺序为高氮型＞高钾型＞均衡型,而钾的肥效期则是高钾型＞高氮型＞均衡型。综上所述,包膜厚度、培养温度及核心肥料同时影响着包膜控释肥料的养分释放特征,养分释放越快,其曲线形状趋向于抛物线型,反之则趋向于S型;3类核心中,以高氮型核心最能发挥水溶性树脂的控释性能。     

热固性树脂包膜控释肥料肥效期的快速预测方法

采用静水溶出率的方法,在25℃、40℃、60℃7、0℃、80℃和100℃条件下,探讨了控释肥料中养分累积释放率与温度的变化规律,以期建立控释肥料肥效期或养分释放期的快速预测方法。结果表明,从低温到高温的各种温度处理下,Scotts公司的Osmocote热固性树脂包膜控释肥料养分累积释放曲线都呈二次曲线,相关指数R2均大于0.996。温度与包膜控释肥料肥效期间呈极显著的负相关,并符合一元二次方程,相关指数R2大于0.993。在高温下培养3或8.h建立的预测预报回归方程,可以快速而准确地预测预报包膜控释肥料在常温下(25℃)的肥效期,预测值与实测值只相差2.4.d;而习惯上的微分溶出率法却相差29～42.d。表明用高温下的肥效期预测预报回归法可以在数小时内准确、迅速地预测控释肥料的肥效期。同时该方法可作为控释肥料在线生产质量控制和市场上控释肥料质量检验的候选方法。     

Nitrogen use efficiency with the application of controlled release fertilizers coated with Kraft pine lignin

The aim of the present paper is to assess the efficiency of several experimental fertilizers in a soil-plant system. The laboratory-prepared fertilizers consisted of granular urea coated with Kraft pine lignin. Five fertilizers were used with coatings differing in thickness and/or the addition of linseed oil as a sealing agent. The experiment was carried out in pots inside a glasshouse. The crop used was rye-grass. Results were compared with those from a urea control treatment without coating and a soil without fertilizer application.

The dry matter yield and the N uptake by the plant were higher in the treatments with coated controlled release fertilizers (CRF) than in those with uncoated urea. There was a lower nitrogen loss through leaching when using CRF (34 to 68%) was used than when using uncoated urea (over 74%) was used. The N use efficiency was lower for urea than for coated fertilizers. This index increased with the thickness of the coating and the addition of the sealing agent.     

膜材料及其构成对调节控释肥料养分释放特性的影响

试验采用水溶出率实测法研究了自行研制的控释肥料养分释放的特性。以养分释放速率和释放期为主要指标评价了膜材料及其构成对调节控释肥养分释放特性的影响。结果表明,膜材料M2的控释性能优于膜材料M1;用膜材料M1包膜肥料的养分累积释放曲线呈对数曲线,而用膜材料M2包膜肥料的养分累积释放曲线呈直线型。在膜的比面重(单位肥料面积上所含膜材料的重量)为20～80g/m2范围内,随着比面重的增加,包膜肥的初期溶出率降低,释放期延长;通过调节膜材料组成与比面重可以研制出释放期不同的控释肥料。     

超微细磷矿粉包膜缓释肥的缓释特征及其对大白菜生理特性的影响

以超微细磷矿粉为主要膜材料对普通复合肥(N-P2O5-K2O:15-15-15)进行包膜,制备了超微细磷矿粉分别占膜材料质量0%、40%、50%和60%比例的4种包膜缓释肥料,分别为CRF2、CRF3、CRF4、CRF5。通过室内养分缓释性能试验和大田试验研究了超微细磷矿粉包膜肥养分缓释特征及其对大白菜生理特性的影响。结果表明:1)用日产JEM-1200EX型电镜扫描观察膜形态结构,4种比例的超微细磷矿粉包膜复合肥随膜材中超细磷矿粉比例的增加其膜壳表面均匀度和致密度增强,对养分释放的缓释能力逐步增强,但缓释效果较树脂包膜肥略差。4种自制包膜肥的养分释放期较普通复合肥延长58～68d,但低于释放期为88天的树脂包膜肥。4种自制包膜肥在土壤培养试验中的土壤氮素表观释放率与树脂膜接近。2)与普通复合肥相比,4种自制包膜肥,能不同程度提高大白菜中后期叶绿素含量、净光合速率(Pn)、蒸腾速率(E)等,提高结球期根系活力及叶片的超氧化物歧化酶(SOD)、过氧化氢酶(CAT)、过氧化物酶(POD)等酶的活性。同时,大白菜单株的结球质量增加0.17～0.77㎏,产量提高6.66%～35.50%,提高了收获期大白菜的含糖量、糖酸比以及维生素C(VC)含量;3)与树脂包膜复合肥相比,各项生理指标均无显著差异。4种自制包膜肥的缓释性能及改善大白菜生理特性的顺序均为:CRF5≈CRF4>CRF3>CRF2。     

磷酸氢钙包膜尿素的研制及其释放特性

以聚乙烯醇水溶液为粘结剂,以肥料级磷酸氢钙为包膜材料,采用喷雾包涂的方法制备一种新的、多营养的、不污染土壤的缓释/控释尿素。用水浸泡法和土壤培养法表征了包膜尿素的释放特性,用扫描电子显微镜研究了包膜尿素的表面和截面形貌。讨论了涂层量对包膜尿素的缓释性能的影响。实验结果表明:涂层量是影响尿素释放的重要因素,磷酸氢钙包膜尿素在水中氮素的释放行为可用一级释放动力学方程来描述;CU-25和CU-30包膜尿素在水中溶出80%的氮素分别需要5.36.d和12.53.d,而在土壤中溶出80%的氮素所需要的时间大于110.d;包膜尿素的扫描电镜照片显示,包膜层中的缝隙小于1μm。     

Interactions of vitamin D3 with bovine beta-lactoglobulin A and beta-casein

It is of nutritional significance to fortify processed dairy products (e.g., cheese, yogurt, and ice cream) with vitamin D3; however, the inherent complexity of these foods may influence the stability and bioavailability of this nutrient. In the present study, the interactions of vitamin D3 with beta-lactoglobulin A and beta-casein were investigated under various environmental conditions (i.e., pH and ionic strength) using fluorescence and circular dichroism spectroscopic techniques. The results indicated that vitamin D3 was bound to both beta-lactoglobulin A and beta-casein depending on the solution conditions. The apparent dissociation constants ranged from 0.02 to 0.29 microM for beta-lactoglobulin A, whereas the beta-casein apparent dissociation constants ranged from 0.06 to 0.26 microM. The apparent mole ratios were also comparable, i.e., 0.51-2.04 and 1.16-2.05 mol of vitamin D3 were bound per mole of beta-lactoglobulin A and beta-casein, respectively. It was concluded that these interactions may strongly influence vitamin D3 stability and, hence, bioavailability in processed dairy products.     

Linolenic acid-modified chitosan for formation of self-assembled nanoparticles

Chitosan was modified by coupling with linolenic acid through the 1-ethyl-3-(3-dimethylaminopropyyl)carbodiimide-mediated reaction. The degree of substitution was measured by 1H NMR, and it was 1.8%, i.e., 1.8 linolenic acids group per 100 anhydroglucose units. The critical aggregation concentration (CAC) of the self-aggregate of hydrophobically modified chitosan was determined by measuring the fluorescence intensity of the pyrene as a fluorescent probe. The CAC value in phosphate-buffered saline (PBS) solution (pH 7.4) was 5 x 10(-2) mg/mL. The average particle size of self-aggregates of hydrophobically modified chitosan in PBS solution (pH 7.4) was 210.8 nm with a unimodal size distribution ranging from 100 to 500 nm. A transmission electron microscopy study showed that the formation of near spherical shape nanoparticles had enough structural integrity. The loading ability of hydrophobically modified chitosan (LA-chitosan) was investigated by using bovine serum albumin (BSA) as a model protein. Self-aggregated nanoparticles exhibited an increased loading capacity (19.85 +/- 0.04 to 37.57 +/- 0.25%) with an increasing concentration of BSA (0.1-0.5 mg/mL).     

纳米材料胶结包膜型缓/控释肥料对作物产量和品质的影响

为了对纳米级材料胶结包膜型缓/控释肥料的缓/控释性能进行准确的评价,以3年6季作物定位施肥试验为基础,对冬小麦和夏玉米的产量及部分品质进行了监测。结果表明,与等量氮磷钾化肥配施相比,4种纳米级材料胶结包膜型缓/控释肥料不同程度地提高了小麦和玉米子粒产量和蛋白质产量,但蛋白质含量增加不显著,可溶性总糖含量反而降低。纳米级材料胶结包膜型缓/控释肥料对提高冬小麦的产量和品质有一定的促进作用,但不同肥料促进作用大小不同。     

Enzymatic hydrolysis, grease permeation, and water barrier properties of zein isolate coated paper

An inexpensive zein-lipid mixture was isolated from yellow dent, dry-milled corn. Grease permeation through zein isolate applied to brown Kraft paper was found to be independent of loading levels at zein isolate levels above 30 mg/16 in.(2). The data shows that water vapor transmission rates depended on the amount of coating applied. Triacylglycerols were the most abundant lipid in milled corn but were absent in the zein isolate (perhaps due to hydrolysis by lipases). Zein from the paper was hydrolyzed enzymatically and the hydrolysis monitored by SDS-capillary electrophoresis. At an E:S ratio of 1:100 no further increase in the hydrolysate peak occurred after 10 and 30 min for alpha-chymotrypsin and pancreatin 8 x; however, zein and lipid were still present 1 h after hydrolysis by pancreatin 1 x.     

Analysis of fat-soluble vitamins. XXIII. High performance liquid chromatographic assay for vitamin D in vitamin D3 and multivitamin preparations.

Vitamin D is determined in preparations containing other fat-soluble vitamins by high performance liquid chromatography (HPLC). The unsaponifiable residue is extracted and separated from interferences by reverse phase chromatography; the fraction corresponding to vitamin D3 is collected and quantitated using normal phase chromatography (amylalcohol-n-hexane as mobile phase) by measuring the vitamin D3 and pre-vitamin D3 peaks at 254 nm. Previtamin D3 content is calculated as vitamin D3 with a conversion factor (determined on the equipment used). Application of the method to vitamin AD3 mixtures in oils gives 98-102% recovery. The reproducibility, using an external standard, is 2-3%, calculated as the coefficient of variation; with an internal standard, the coefficient of variation is 1-1.5%. The method measures potential vitamin D3 content in preparations containing greater than or equal to 200 IU/g in the presence of all known vitamin D3 isomers, vitamin A, and vitamin E.     

Preparation and comparative release characteristics of three anthocyanin encapsulation systems

Bilberries (Vaccinium myrtillus L.) and their major polyphenolic constituents, anthocyanins, have preventive activities inter alia against colon cancer and inflammatory bowel diseases. However, anthocyanins are sensitive to environmental conditions; thus their bioavailability in the gastrointestinal tract is an important determinant of their in vivo activity. In the study reported here, the potential benefits of encapsulating an anthocyanin rich bilberry extract (BE) on anthocyanin stability were investigated. Nonencapsulated BE and three different BE loaded microcapsule systems were incubated in simulated gastric fluid (SGF) and fed state simulated intestinal fluid (FeSSIF). After exposure to these media, released anthocyanins were identified and quantified by HPLC with UV/Vis detection. Although a rapid release of anthocyanins was observed within the first 20 min, encapsulation of anthocyanins doubled the amount of available anthocyanins after 150 min of incubation. These results illustrate the ability of encapsulation to inhibit early degradation of anthocyanins in the intestinal system.     

纳米材料胶结包膜型缓/控释肥料的特性及对作物氮素利用率与氮素损失的影响

通过冬小麦－夏玉米轮作下3年6季的田间试验,研究纳米级材料胶结包膜型缓/控释肥料对氮素利用率和硝态氮淋溶损失的影响。结果表明,与普通氮磷钾化肥配施相比,4种纳米级材料胶结包膜型缓/控释肥料提高小麦对氮素的利用率2.80～23.38个百分点,玉米对氮素的利用率1.01～21.63个百分点。在0―80 cm土层,PS、BC208和306处理下土壤硝态氮含量高于普通氮磷钾化肥配施处理,而F208处理低于普通氮磷钾化肥配施处理;在80―160 cm土层,均低于普通氮磷钾化肥配施处理;在接近地下水水位土层（140―160 cm）,减少硝态氮1.61～2.42 mg/kg。4种纳米级材料胶结包膜型缓/控释肥料损失出土壤－作物系统的氮素比普通氮磷钾化肥配施处理减少2.00～24.90个百分点。结果表明,纳米级材料胶结包膜型缓/控释肥料能有效的提高氮素利用率和减少硝态氮的淋溶损失。     

Dissolution kinetics of macronutrient fertilizers coated with manufactured zinc oxide nanoparticles

The solubility of Zn in Zn fertilizers plays an important role in the agronomic effectiveness of the fertilizer. On the basis of thermodynamics, zinc oxide (ZnO) nanoparticles (NPs) should dissolve faster and to a greater extent than bulk ZnO particles (equivalent spherical diameter >100 nm). These novel solubility features of ZnO NPs might be exploited to improve the efficiency of Zn fertilizers. In this study, we compared the Zn solubility and dissolution kinetics of ZnO nanoparticles and bulk ZnO particles coated onto two selected granular macronutrient fertilizers, urea and monoammonium phosphate (MAP). The main Zn species on coated MAP and urea granules were zinc ammonium phosphate and ZnO, respectively. Coated MAP granules showed greater Zn solubility and faster dissolution rates in sand columns compared to coated urea granules, which may be related to pH differences in the solution surrounding the fertilizer granules. The kinetics of Zn dissolution was not affected by the size of the ZnO particles applied for coating of either fertilizer type, possibly because solubility was controlled by formation of the same compounds irrespective of the size of the original ZnO particles used for coating.     

微酸性电解水结合壳聚糖对水蜜桃护色保鲜的效果

为了防止水蜜桃(Prunus persicaL.Batsch)采后的果肉颜色变化而严重影响其商品价值。该研究以南汇水蜜桃为材料,分别利用自制羧甲基壳聚糖复合保鲜剂,以及微酸性电解水对水蜜桃进行护色保鲜处理,并对冷藏条件下(2℃)水蜜桃果肉颜色及与颜色品质变化相关的指标进行了检测,同时还利用核磁共振成像(MRI)合成T2-MAP图研究了冷藏开始和结束后水蜜桃内部变化的规律。结果表明,在贮藏结束后,对照组果肉颜色的L*值、H*值、C*值分别是羧甲基壳聚糖复合保鲜剂和微酸性电解水处理组的85%～91%、85%～93%和114%～122%(p<0.05)。显然,羧甲基壳聚糖复合保鲜剂和微酸性电解水由于可以抑制水果自身乙烯的产生,减少水果的细胞膜透性和T2-MAP图中T2弛豫常数的变化,降低了多酚氧化酶(PPO)活性的增加速度,减少了酚类物质的累积,进而延缓了果肉的变色。另外,与仅用电解水处理相比,结合羧甲基壳聚糖处理具有较好的护色保鲜效果。通过该研究,可以为提高采后南汇水蜜桃的果肉护色保鲜效果提供参考。