响应面法优化微胶囊复合壁材配比

采用高压静电微胶囊制备装置,以成囊合格率为检测指标,选择海藻酸钠等为壁材,运用Box-Behnken中心组合设计和响应面分析,研究了壁材配比对微胶囊特性的影响。得到的最优条件是:壁材组成为质量分数1.53%(以下都是质量分数)海藻酸钠,4.52%聚乙烯醇,1%明胶,1%甘油,成囊溶液氯化钙质量浓度为22.86g/L,微胶囊合格率为87.37%。在最优条件下制备出的微胶囊内外表面光滑,囊壁透明,分散性好,形态完整。可为食品、医药、化工等微胶囊化壁材配比选择提供参考。     

薄荷油微胶囊的制备及其共混熔融纺丝

以密胺树脂为壁材、薄荷油为芯材制备薄荷油微胶囊并与聚丙烯(PP)进行熔融共混纺丝得到了芳香纤维。通过设计正交试验,获得微胶囊的最佳制备工艺条件为:芯壁质量比2∶3、壁材质量分数8%、乳化剂质量分数0.8%、缩聚时间2 h;所得的微胶囊平均粒径小(4.568μm)、热稳定性好、形貌规整且产率高(63.17%)。以PP为基体制备微胶囊质量分数20%的母粒,再与PP进行共混熔融纺丝,结果表明:当共混物中微胶囊的实际添加质量分数为2.5%时,共混物可纺性好,纤维的强度可达3.4 c N/dtex。在纺丝前后微胶囊的含油率变化不大,纤维中的含油量为14.05 mg/g。     

溶剂蒸发法制备高效氯氟氰菊酯微胶囊及性能

以乙基纤维素为壁材、二氯甲烷为溶剂,采用溶剂蒸发法制备了高效氯氟氰菊酯微胶囊。通过单因素实验考察了溶剂质量分数、壁材质量分数、乳化剂质量分数和剪切时间对微胶囊平均粒径的影响,通过以微胶囊平均粒径和未包封率作为评价指标的正交实验L9(34)优选了最佳工艺,并通过SEM、FTIR和HPLC对微胶囊的外观形貌、包覆效果和释放性能进行了表征。结果表明:随着溶剂质量分数增大,微胶囊平均粒径先减小后增大,w(溶剂)=25%时,平均粒径最小。随着壁材质量分数增大,微胶囊平均粒径增大。随着乳化剂质量分数增大,微胶囊平均粒径逐渐减小。固定剪切速率,微胶囊平均粒径随着剪切时间增加而减小。以w(二氯甲烷)=25%、w(乙基纤维素)=0.75%、w(乳化剂)[m(Tween80)∶m(Span20)=5∶1]=2%、剪切时间为8 min的工艺条件下得到的微胶囊外观光滑,形态规则,粒径较小(约19.2μm)且均匀,包封率高达82.8%,且具有较好的缓释性能。     

纳米SiO_2改性脲醛树脂/十二醇相变微胶囊的制备及性能

利用原位聚合法制备了以纳米SiO_2改性脲醛树脂为壁材、十二醇为芯材的相变微胶囊。考察了芯壁质量比、固化终点pH和纳米SiO_2质量分数对微胶囊包封率和芯材质量分数、渗透率的影响,采用扫描电子显微镜(SEM)、差示扫描量热仪(DSC)和热重分析仪(TG)等分别对微胶囊相变材料的表面形貌、粒径和热性能进行了表征。研究结果表明,纳米SiO_2改性脲醛树脂/十二醇相变微胶囊的最佳制备条件为:芯壁质量比为1∶2、固化终点p H=1.5~2、纳米SiO_2质量分数为3%。制备的微胶囊为表面光滑的球形,粒径大小为1.85~5μm,包封率和芯材质量分数分别为62.5%和79.3%,相变潜热为148.4 J/g。     

茶油微胶囊的制备及其缓释性能研究

为提高茶油的存储稳定性，以乳清分离蛋白(WPI)与阿拉伯胶(GA)为复合壁材，转谷氨酰胺酶为固化剂，采用复凝聚法制备茶油微胶囊。首先，以凝聚率为指标，通过单因素实验确定最佳的壁材复凝聚参数；随后，以微胶囊形貌和包埋率为指标，通过单因素实验和响应面实验确定最佳的茶油微胶囊制备条件：壁材质量分数2.0% 、壁材组分WPI与GA的质量比1:1、芯壁质量比0.84:1、复凝聚pH=4.3、复凝聚温度40 ℃和搅拌速度500 r/min，此时包埋率达89.67%。红外光谱、扫描电镜、粒度分布、休止角、POV值和热重分析结果表明，茶油微胶囊结构完整、粒径均一且具有良好的流动性、分散性、热稳定性和抗氧化性。体外缓释数据表明，茶油微胶囊在模拟胃液和肠液中的缓释机理均符合Ritger-Peppas缓释模型，符合人体消化吸收特性。茶油微胶囊化保护茶油的有效成分，扩展其使用范围，提高其消化吸收效果。     

艾叶提取物驱蚊微胶囊的制备

以天然驱蚊植物——艾叶提取物为芯材,采用复相乳液法制备驱蚊微胶囊。讨论了初乳中乳化剂用量、芯材与二氯甲烷体积比、壁材用量、保护性胶体浓度等对微胶囊粒径的影响,获得了最佳制备工艺。将粒径最小的微胶囊与黏合剂以一定比例混合后整理到涤纶织物上,并对驱蚊效果进行测试和分析。结果表明:最佳制备工艺为初乳中乳化剂体积分数为6%,芯材与二氯甲烷体积比为1∶6,壁材质量分数为4%,保护性胶体质量分数为2%;制得的微胶囊最小平均粒径为2.78μm;整理到涤纶织物上的驱蚊效果显著,蚊虫驱避率达到70%。     

原位聚合法制备分散染料微胶囊

以尿素和甲醛为壁材,分散染料酸性红GP(C.I.266)为囊芯制备了分散染料微胶囊。用SEM和Zeta激光粒度测定仪观察分析微胶囊的粒径分布,讨论了反应条件对微胶囊粒径分布的影响。通过实验,提出了制备该分散染料微胶囊的最佳反应条件为:壁材n(尿素)∶n(甲醛)=2∶3,分散剂阿拉伯树胶质量分数为5%,m(芯材)∶m(壁材)∶m(分散剂)=1∶7 25∶2 5,在pH=3,80℃和搅拌速率为1500r/min的体系中反应2h。     

水酶法提取显齿蛇葡萄籽油及其微胶囊化研究

以显齿蛇葡萄籽为原料,通过单因素试验和响应面分析法对水酶法提取显齿蛇葡萄籽油的工艺进行研究。结果表明,水酶法提取显齿蛇葡萄籽油的较佳工艺为:液料比(m L/g)为12.6,中性蛋白酶的质量分数为1.4%,酶解温度为52.0℃,酶解时间为3.2 h,此条件下显齿蛇葡萄籽油提取率达到10.30%。以大豆分离蛋白和麦芽糊精为壁材,通过正交试验对显齿蛇葡萄籽油微胶囊化的工艺进行研究。结果显示,显齿蛇葡萄籽油微胶囊化的较佳条件为:壁材的质量分数为13%,芯材壁材质量比为1∶6,喷雾干燥器进、出风口温度分别为125和62℃,均质压力为28 MPa,此条件下显齿蛇葡萄籽油微胶囊化包埋率为92.3%。     

纳米纤维素改性相变储能材料的制备与表征

以石蜡为芯材,纳米纤维素(CNFs)改性的三聚氰胺-尿素-甲醛树脂(MUF)为壁材,采用原位聚合法制备了纳米相变微胶囊。采用红外光谱仪、示差扫描量热仪、热重分析仪和场发射扫描电镜(FE-SEM)等对产物的性能进行了分析和表征。结果表明,加入质量分数1.5%的CNFs时,CNFs在壁材中分布均匀,制备的石蜡微胶囊相变焓达61.20 J/g,使得微胶囊的包含量从50.1%升高到55.6%,破损率从30.2%下降到24.5%。     

掺杂纳米-TiO_2改性相变微胶囊壁的性能研究

以掺杂金属Fe~(3+)、Zr~(4+)、Ce~(4+)的TiO_2纳米粒子及TiO_2纳米粒子填充聚乙烯醇(PVA)改性密胺甲醛树脂为微胶囊复合壁材,以十四烷为芯材,采用原位聚合法制备了掺杂TiO_2纳米粒子填充PVA改性囊壁的相变微胶囊。考察了掺杂TiO_2纳米粒子对微胶囊机械性能、热性能及表面形态的影响,采用FT-IR、TG和SEM等方法对其进行了表征。结果表明,当囊壁中均匀地掺杂纳米TiO_2后,微胶囊的机械强度增大,芯材释放率减小。当壁材中Fe~(3+)掺杂纳米TiO_2质量分数为0.5%时,微胶囊破损率为18.5%,芯材10 d释放率为22.6%。     

共轭亚油酸粉末化微胶囊的制备

研究了喷雾干燥法制备共轭亚油酸微胶囊的工艺参数及配比条件。结果表明,最佳的工艺参数及配比条件为:乳液80℃热处理60 m in,乳化剂蔗糖酯加入量为水液的1%~1.5%,大豆分离蛋白与麦芽糊精质量比为1∶4,壁材中玉米糖浆含量38.5%,固形物含量16.7%,共轭亚油酸理论含量16%左右,进风温度130~150℃,进料流量(2.5~3.5)×150 mL/h,进料温度35℃,进风流量1.1 m3/m in左右,喷嘴压力180 kPa。制备出的共轭亚油酸微胶囊有较好的产品质量。     

Microencapsulation of capsanthin by soybean protein isolate‐chitosan coacervation and microcapsule stability evaluation

Although capsanthin possesses excellent coloring performance and healthcare functions, its application in the food industry is limited due to its susceptibility to humidity, heat, and light. The purpose of this research was to microencapsulate capsanthin by soybean protein isolate (SPI)‐chitosan coacervation and evaluate whether the microencapsulation improved the stability of capsanthin against the adverse conditions mentioned above. The results indicated that the optimum conditions for capsanthin microencapsulation were emulsification speed 10,000 rpm, emulsification temperature 45°C, wall concentration 15 g/L and core to wall ratio 1:2 (w/w). Under these conditions, the droplets in the emulsion were even in size distribution without agglomeration and the microencapsulation efficiency and microencapsulation yield reached 90.46% and 86.69%, respectively. Microencapsulation increased the stability of capsanthin against low/medium moisture, heat, and especially light, but was less effective in protecting capsanthin microcapsules in high moisture. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39671.     

共轭亚油酸乙酯的合成

采用间歇式反应 ,以硫酸、磷酸、对甲苯磺酸为催化剂对共轭亚油酸乙酯进行了合成 ,并采用正交实验设计研究了物料比、反应温度、反应时间、催化剂用量对产品收率和品质的影响。硫酸、对甲苯磺酸催化活性佳 ,磷酸催化活性差。得到了如下合成工艺条件 :硫酸催化 ;n(共轭亚油酸 )∶n(无水乙醇 ) =1∶6;酯化反应温度 76℃ ;反应时间 1h ;催化剂用量为共轭亚油酸质量的 2 5 % ,收率可达 75 % ,产品w(共轭亚油酸乙酯 ) =77%～ 82 %。     

酯交换法合成共轭亚油酸三甘酯

采用酯交换反应,以共轭亚油酸乙酯、甘油为原料,脂肪酸钾为均相化试剂,无水K2CO3为催化剂,在压力～1 0kPa下反应制得共轭亚油酸三甘酯。合成工艺条件:n(共轭亚油酸乙酯)∶n(甘油)=6∶1;酯化反应温度140℃;反应时间～1 5h;无水K2CO3用量为共轭亚油酸乙酯质量的0 5%～1%;按统计平均值,产物三甘酯脂肪酸侧链中w(共轭亚油酸)>80%;产率(以甘油计)60%～65%。     

The Efficacy of Compounds with Different Polarities as Antioxidants in Emulsions with Omega-3 Lipids

According to the so-called polar paradox hypothesis, the efficacy of an antioxidant in emulsions is highly affected by its polarity and thereby location in the different phases. However, other factors also affect the efficacy of antioxidants in multiphase systems. The aim of this study was to evaluate the efficacy of antioxidants [ascorbic acid, ascorbyl palmitate, ascorbyl CLA and CLA (conjugated linoleic acid)] with different polarities in two different emulsion systems: o/w emulsion (5% oil) and w/o emulsion (98% oil) stabilized with citrem and PGPR, respectively. The efficacy of the antioxidants was compared to their partitioning in an o/w emulsion system and to results obtained from different antioxidant assays: iron reducing power, chelating activity and radical scavenging activity. For the w/o emulsions the efficacy of the antioxidants followed the polar paradox hypothesis: ascorbyl palmitate = ascorbyl CLA > ascorbic acid ≥ CLA > reference. For the o/w emulsion the antioxidative effects were not in accordance with the polar paradox. In the beginning of the storage, ascorbyl palmitate and ascorbic acid were most efficient, however in the end they acted as prooxidants. Ascorbyl CLA was located at the interface but was inactive as an antioxidant. This may be due to impurities or interaction with citrem.     

Oxidative stability of blends and interesterified blends of soybean oil and palm olein

Improvement of oxidative stability of soybean oil by blending with a more stable oil was investigated. Autoxidation of blends and interesterified blends (9∶1, 8∶2, 7∶3 and 1∶1, w/w) of soybean oil and palm olein was studied with respect to fatty acid composition, fatty acid location and triacylglycerol composition. Rates of formation of triacylglycerol hydroproxides, peroxide value and volatiles were evaluated. The fatty acid composition of soybean oil was changed by blending. Linolenic and linoleic acids decreased and oleic acid increased. The triacylglycerol composition of blends and interesterified blends was different from that of soybean oil. Relative to soybean oil, LnLL, LLL, LLO, LLP, LOO and LLS triacylglycerols were lowered and POO, POP and PLP were higher in blends and interesterified blends (where Ln, L, O, P and S represent linolenic, linoleic, oleic, palmitic and stearic acids, respectively). Interesterification of the blends leads to a decrease in POO and POP and an increase in LOP. Linoleic acid concentration at triacylglycerol carbon-2 was decreased by blending and interesterification. Rates of change for peroxide value and oxidation product formation confirmed the improvement of soybean oil stability by blending and interesterification. But, blends were more stable than interesterified blends. Also, the formation of hexanal, the major volatile of linoleate hydroperoxides of soybean oil, was decreased by blending and interesterification.     

脂肪酸盐用于反相乳液中淀粉接枝反应乳化剂的研究

研究了以淀粉为基材、以丙烯酰胺(AM)和二甲基二烯丙基氯化铵(DMDAAC)为聚合单体、以脂肪酸盐及其复配物为乳化剂、采用反相乳液聚合技术合成接枝共聚物的方法。讨论了脂肪酸盐的金属离子种类、碳链长度、乳液形成方法、乳化剂组成、乳化剂用量对单体转化率、接枝率、接枝效率、产品特性黏数及絮凝效果的影响。结果表明,将单一的脂肪酸盐以一定比例进行复配得到的混合物的乳化效果较好,当m(油酸)∶m(油酸钠)=60∶40的复配物为乳化剂,w(乳化剂)=6%,V(油)∶V(水)=1 2∶1,n(AM)∶n(DMDAAC)=3∶1,c〔(NH4)2S2O8〕=3 5×10-4mol/L,t=6h,θ=45℃时,单体转化率达99 7%,接枝率达97 6%,接枝效率为97 9%,特性黏数为1120mL/g。     

Antioxidant behaviour of products resulting from beef sarcoplasmic proteins‐malondialdehyde reaction

The antioxidant properties of the soluble fraction of a Maillard reaction product (MRP) model generated from sarcoplasmic protein/malondialdehyde (MDA) were evaluated. The dry extract colour values showed that it has a pale brown colour appearance, and the carbonyl content of isolated protein increased from 2474 nmol/mg protein to 3904 nmol/mg protein, before and after reaction with MDA, respectively. Reducing power (82.34%) and 1,1‐diphenyl‐2‐picryl hydrazyl radical scavenging (35.20%) were very good, while superoxide anion scavenging showed poor inhibition (324 equivalent SOD units/g). Antioxidant activity in the fused lard system was stronger than in the emulsion system, on all parameters tested, exerting 89% reduction on hydroperoxides, 78% on thiobarbituric acid‐reactive substances (TBARS) and 69% on conjugated dienes (CD) at 80 °C. In the linoleic acid/water emulsion system, the antioxidant activity, measured as peroxide formation inhibition at 37 °C, at the higher concentration assayed was 81%, whereas on CD and on TBARS, it exerted a moderate inhibition (45% and 58%). At 80 °C, the antioxidant activity, for the same concentration, was less effective (37% on CD; 75% on peroxide values, and 40% on TBARS). In conclusion, the sarcoplasmic protein/MDA reaction products showed an excellent antioxidant activity in fused lard and a good performance in the linoleic/water emulsion system.     

高纯度共轭亚油酸的规模化制备及其异构体的鉴定

Conjugated linoleic acid(CLA)is a kind of fatty acid with physiological activities and potential appli-cation prospect ,A synthesis method of conjugated linoleic acid and a purification technology were studied .CLA was prepared and purified by urea-complexation and conjugation using safflower oil as raw material,The purity of CLA and total recovery of the product was more than 95% and 48%,respectively,The main isomers produced in alkali-catalyzed conjugation were identified by gas chromatography (GC)linked to mass spectrometry(MS) and Fourier transform infrared spectroscopy(FTIR),The total amount of the two main isomers (9cis,11trans-and 10trans,12cis-CLA) determined by GC was more than 90% of the product.     

Synthesis and characterization of polyurea microcapsules containing essential oils with antigerminative activity

In this paper we report on the preparation and characterization of polyurea‐based microencapsulated systems, containing essential oils as core materials, for potential applications in controlled‐release formulations of agrochemicals. Microcapsules were synthesized by interfacial polymerization in o/w emulsion between polyfunctional isocyanates and diamines, to investigate the effect of the monomer kind on the morphology and properties of the produced samples. The synthetic conditions that gave the best results were used to microencapsulate four essential oils, able to interfere with the seed germination and radicle elongation of some test plants. The produced samples were characterized, with the aim to analyze their morphology and to verify the effectiveness of essential oil microencapsulation. Moreover, preliminary bioassay based on seed germination and subsequent radical growth were carried out to study the effects of the microencapsulated essential oils. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007