Enhanced water-solubility of Licorice extract microparticle prepared by antisolvent precipitation process

In this study, Licorice extract (LE) microparticles were successfully prepared using antisolvent precipitation process. Ethyl acetate and dimethyl sulfoxide, were used as the antisolvent and solvent, respectively. By means of orthogonal experimental design, the influences of several process parameters on the mean particle size (MPS) were investigated. The concentration range of the LE solution, the volume ratio of solvent to antisolvent, dripping speed, and temperature were 4.3–34.5 mg/mL, 1:1–1:12, 1–10 mL/min, and 20–35 °C, respectively. Based on the above orthogonal experiments, the optimum antisolvent precipitation process conditions were found to be: temperature 20 °C, concentration of the LE solution 17.2 mg/mL, volume ratio of solvent to antisolvent 1:4, dripping speed 10 mL/min. The LE microparticles were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TG), differential scanning calorimetry (DSC), HPLC analysis and dissolution test. And the morphology, crystalline state and chemical structure, drug purity, dissolution rate and bioavailability of LE microparticles were investigated. Under optimum antisolvent precipitation process conditions, the MPS of LE microparticles reached to 85.3 nm, and with uniform distribution. And the LE microparticles had the same chemical structure as the unprocessed drug, but the crystallinity was reduced, purity was increased. Furthermore, the water solubility increased from 4.82 mg/mL to 16.10 mg/mL, and bioavailability is increased by 64.36%.     

水性聚氨酯制备工艺对乳液黏度和胶粒尺寸的影响

以异佛尔酮二异氰酸酯(IPDI)、聚四氢呋喃醚二醇(PTMG)、聚己内酯二醇(PCLD)、2,2-二羟甲基丙酸(DMPA)以及1,4-丁二醇等为主要原料,经自乳化法分别制备出IPDI型水性聚氨酯PTMG-PU、PCLD-PU。红外光谱(FT-IR)测试证实了二者结构上的差别。通过研究合成制备工艺过程中多种因素对乳液黏度及胶粒粒径的影响,发现当控制中和度为90%~100%、n(NCO)/n(OH)比为1.13~1.20、DMPA质量分数为2.5%~9.0%以及乳化时叶片转速为1500 r/min~2000 r/min、加水速度为100 mL/min~200 mL/min(体系总体积200 mL)时,可制得乳液黏度和胶粒粒径适中且固含量可达40%以上稳定的IPDI型聚氨酯乳液。     

Preparation of superfine ammonium perchlorate particles using some advanced liquid antisolvent crystallization (LASC) methods

The aim of this study is to investigate the crystallization of superfine ammonium perchlorate (AP) particles using some advanced liquid antisolvent crystallization (LASC) methods containing liquid antisolvent equipped with Y-jet mixer (LASY) and evaporation antisolvent crystallization (EASC) methods. Scanning electron microscopy (SEM), optical microscopy and X-ray diffraction techniques were used to investigate the crystal-size distribution (CSD), average particle size (APS), sphericity, uniformity coefficient (UC), and crystallinity of prepared samples. Also, microstructure image processing (MIP) technique in combination with MATLAB and the Rosin–Rammler (RR) equation were used to analyze specifications of the prepared particles. The results of MIP analysis technique were illustrated that the particles obtained with the LASY method represented higher sphericity (0.89–0.92) than EASC method (0.79–0.82). Also according to the Rosin–Rammler analysis results, the highest uniformity coefficient was related to the LASY method (3.83–4.02). The results of this study were shown that the LASY method can be considered as a safe and simple procedure for rapid preparation of superfine ammonium perchlorate particles with regular morphology.     

微波辐射下交联壳聚糖微球的制备及吸附性能研究

微波辐射下,以壳聚糖为原料,甲醛为预交联剂,环氧氯丙烷为交联剂,制得甲醛环氧氯丙烷交联壳聚糖微球树脂,研究了合成条件对微球吸附性能的影响,并采用傅里叶红外光谱仪和电子扫描电镜对树脂的微观结构和形貌进行表征。结果表明,树脂具有很好的球形;Shiff碱反应能够很好地保护壳聚糖上的氨基;交联剂用量、搅拌速率和酸处理条件对树脂的吸附性能的影响较大。当合成条件为搅拌速率600r/min、甲醛1.5mL、环氧氯丙烷3mL、酸化时间8min、盐酸用量30mL,所得交联壳聚糖微球对Cu(Ⅱ)的吸附容量可达到269.83mg/g。     

Estimation of three‐dimensional stress intensity factor for structural ‘T’ details

Three‐dimensional (3D) opening mode stress intensity factors (SIFs) for structural steel‐welded ‘T’ details were investigated by the finite element method. A 3D shape‐dependent correction factor is proposed for semi‐elliptical surface cracks. The aspect ratio (a/c) of a semi‐elliptical crack plays a key role in the approximation of 3D‐SIF values, and in the present study, it was estimated for a 3D crack analysis. The estimated 3D‐SIF was determined through a correlation between the a/c ratio and the two‐dimensional SIF for semi‐elliptical cracks in the thickness direction adjacent to the web‐flange junction of a welded ‘T’. The resulting equation can be used to estimate the 3D‐SIF values from the two‐dimensional SIF without much ambiguity.     

Modified supercritical antisolvent method with enhanced mass transfer to fabricate drug nanoparticles

The main aim of this study was to modify the supercritical antisolvent precipitation method to enhance the mass transfer in order to prepare smaller nanoparticles of drugs. The supercritical antisolvent apparatus was customized by introducing a titanium horn in the precipitation chamber for generation of the ultrasonic field for enhanced mass transfer and the method was called supercritical antisolvent with enhanced mass transfer (SAS-EM). The effects of flow rate, ultrasonic amplitude, drug concentration and flow time on the particle size were investigated. The results showed that increasing the flow rate, incrementing the ultrasonic power up to an optimum point, decreasing the drug concentration and reducing the flow time helped to achieve smaller quercetin particles in the range of 120–450 nm. It is also shown that there is a tradeoff between the particle size and the yield; therefore the process parameters can be selected based on the particle size requirement. DSC studies suggested that the crystallinity of SAS-EM prepared quercetin nanoparticles decreased as compared to original quercetin powder. The dissolution of SAS-EM prepared nanoparticles increased significantly in comparison with the original quercetin powder. However, there was no significant difference in the dissolution of various quercetin nanoparticles samples prepared by the SAS-EM process. The best dissolution percent achieved was 75% for the smallest size sample prepared at the flow rate of 5 ml/min, power supply of 200 W, drug concentration of 10 mg/ml, and flow time of 4 min.     

Preparation and in vitro/in vivo evaluation of gliclazide loaded Eudragit nanoparticles as a sustained release carriers

The aim of this study was to formulate and optimize gliclazide-loaded Eudragit nanoparticles (Eudragit L100 and Eudragit RS) as a sustained release carrier with enhanced efficacy. Eudragit L 100 nanoparticles (ELNP) were prepared by controlled precipitation method whereas Eudragit RSPO nanoparticles (ERSNP) were prepared by solvent evaporation method. The influence of various formulation factors (stirring speed, drug:polymer ratio, homogenization, and addition of surfactants) on particle size, drug loading, and encapsulation efficiency were investigated. The developed Eudragit nanoparticles (L100 and RS) showed high drug loading and encapsulation efficiencies with nanosize. Mean particle size altered by changing the drug:polymer ratio and stirring speed. Addition of surfactants showed a promise to increase drug loading, encapsulation efficiency, and decreased particle size of ELNP as well as ERSNP. Dissolution study revealed sustained release of gliclazide from Eudragit L100 as well as Eudragit RSPO NP. SEM study revealed spherical morphology of the developed Eudragit (L100 and RS) NP. FT-IR and DSC studies showed no interaction of gliclazide with polymers. Stability studies revealed that the gliclazide-loaded nanoparticles were stable at the end of 6 months. Developed Eudragit NPs revealed a decreased t_min (ELNP), and enhanced bioavailability and sustained activity (ELNP and ERSNP) and hence superior activity as compared to plain gliclazide in streptozotocin induced diabetic rat model and glucose-loaded diabetic rat model. The developed Eudragit (L100 and RSPO) NP could reduce dose frequency, decrease side effects, and improve patient compliance.     

Fatigue crack growth simulation in a first stage of compressor blade

A first-stage rotary compressor blade of a Model GE-F6 gas turbine failed due to vibration in early March 2008. Initial investigations showed that pitting on the pressure side of the blade caused micro cracks, leading to larger cracks due to high cycle fatigue. To assess this failure, a series of experimental, numerical, and analytical analyses were conducted. Fractography of the fractured surface of the blade indicated that two semi-elliptical cracks incorporated and formed a single crack. In this study, static and dynamic stress analyses were performed in Abaqus software. Moreover, fracture mechanics criterion was accomplished to simulate fatigue crack growth. This was carried out using a fracture analysis code for 3-dimensional problems (Franc3D) in two states. Firstly, stress intensity factors (SIFs) for one semi-elliptical surface crack and then SIFs for two semi-elliptical surface cracks were taken into account. Finally, the Paris and Forman–Newman–De Koning models were used to predict fatigue life. Since stress level and crack shape in both conditions are the same and the SIF at the crack tip reaches the fracture toughness of the blade, SIFs results indicate that insertion of a second crack has no effect on the final SIF, however, the second crack facilitates the process of reaching the critical length. So, fatigue life in two-crack condition is less than in the one-crack state.     

非均匀成核法制备硅酸铝-硅灰石复合粉体材料

以硅灰石为原料,硫酸铝和硅酸钠为包覆剂,采用非均匀成核法制备一种硅酸铝-硅灰石复合粉体材料,研究搅拌速度、反应温度、反应时间、硫酸铝溶液浓度和滴加速度等工艺条件对复合粉体制备的影响。结果表明,控制机械搅拌速度为300~400 r/min,反应温度为80℃,反应时间为30 min,硫酸铝溶液浓度为0.1 mol/L,滴加速率为1~2 mL/min,可以实现硅酸铝以非均匀成核形式沉积在硅灰石表面,包覆硅酸铝后硅灰石白度提高,粒度增大,比表面积提高200%以上。     

超临界抗溶剂法制备聚乳酸微球

采用超临界抗溶剂技术,对影响聚乳酸(PLA)微球粒径的溶液浓度和溶剂配比进行了初步研究。在温度38℃、压力10 MPa、溶液流速1.0mL/min、喷嘴直径300μm条件下,研究不同溶液浓度和溶剂配比对聚乳酸微粒粒径和粒径分布的影响。结果表明:当聚乳酸质量浓度为10 mg/mL、混合溶剂二氯甲烷和丙酮的体积比为V(CH_2:Cl_2):V(CH_3COCH_3)=1:2时效果最好,得到的粒堆松软,粒径集中在530～950 nm,粒径分布窄,吹干只需12 min。     

Mg_2Si/AZ91D复合材料阻尼性能

以AZ91D镁合金为基体,采用搅熔铸造法将球磨后的粉煤灰漂珠颗粒加入到熔融态基体中,设置球磨漂珠质量分数(2%、6%和10%)和搅拌时间(3min和6min),成功制备了Mg2Si/AZ91D复合材料。采用金相分析、XRD分析和动态机械热分析等方法研究了铸态和固溶态Mg2Si/AZ91D复合材料的显微组织、成分及阻尼性能。研究表明:与AZ91D镁合金相比,加入球磨漂珠颗粒后制备的Mg2Si/AZ91D复合材料中生成了Mg2Si相,而且随着漂珠质量分数的增加,Mg2Si相呈现不规则形状,固溶后Mg2Si相呈现均匀块状。随着漂珠质量分数的增加,Mg2Si/AZ91D复合材料的阻尼性能越好,搅拌时间6min制备的复合材料阻尼性能高于搅拌时间3min制备的复合材料的阻尼性能,并且固溶态的阻尼性能优于铸态。在室温下,Mg2Si/AZ91D复合材料阻尼性能可用位错理论来解释。     

Development of α-Tocopherol Acetate Nanoparticles: Influence of Preparative Processes

We studied different methods of preparing α-tocopherol acetate (ATA) nanoparticles, which are to be used in targeting the lungs as aerosols in order to prevent cigarette smoke toxicity. Poly-(lactide) nanoparticles were prepared using nanoprecipitation and solvent evaporation techniques, which produced, respectively, too small and too large nanoparticles to be aerosolized. The emulsification-diffusion method produced 2 months stable nanoparticles with a size between (500–700 nm). Increasing ATA concentration (1–7 mg/mL) induced a decrease in the association rate (97–93%) and in the adsorbed ATA rate (7–4.5%), which was associated with variations of Zeta potentials (?27.5 to ?24.3 mV) and decrease in polymeric wall thickness and density.     

乙醇和磁搅拌对高压制备阳极氧化铝膜的影响

硬质阳极氧化(HA)过程中添加乙醇和使用磁搅拌能够有效抑制烧穿现象的发生。将0.3mol/L草酸电解液的溶剂设置为体积比分别为1:1、2:1、3:1和4:1的去离子水与乙醇混合溶液,同时使用磁搅拌进行二次高压阳极氧化。通过分析电流时间曲线和原子力显微镜(AFM)表征的表面形貌,研究了乙醇添加量和磁搅拌对高压阳极氧化的影响。结果表明:溶剂中水与乙醇体积比的大小对制备出模板的孔径和孔间距几乎没有影响;氧化过程中及时改变磁搅拌速度可以有效抑制烧穿现象,使用变速磁搅拌也可制备出高有序度的阳极氧化铝模板。     

溶剂挥发法制备苯乙烯微胶囊

采用简单易控制的溶剂挥发法成功制备了聚砜材料包覆苯乙烯的自修复微胶囊,通过核磁共振氢谱(1H-NMR)、扫描电子显微镜(SEM)、元素分析仪和热重分析仪(TGA)对微胶囊的化学结构、表面形貌及其热性能进行了研究.结果表明,选择0.5％的聚乙烯醇表面活性剂,700 r/min乳化转速、芯壁比2∶1时制得的微胶囊表面光滑,体积平均粒径为120μm,并且分布比较窄,微胶囊在室温下具有一定缓释性.     

Formation of PLLA-PEG-PLLA Microparticles by Supercritical Antisolvent Process

A biodegradable triblock copolymer of poly(L-lactide)–poly(ethylene glycol)–poly(L-lactide) (PLLA-b-PEG-b-PLLA) was synthesized via a new process by the ring-opening polymerization of L-lactide with PEG as macroinitiator and Sn(Oct)₂ as catalyst. The structure and molecular weight of the polymer were characterized by ¹H NMR spectra, Fourier transform infrared spectroscopy (FTIR), and gel permeation chromatography (GPC). Then the microparticles were prepared with the synthesized copolymer by supercritical antisolvent (SAS) process. The optimal operating conditions were explored using an orthogonal array design. The effects of the mixed organic solvent, the concentration of polymer solution and the flow rate of polymer solution on the morphology and thermal properties of the microparticles were investigated experimentally. The morphology, size and thermal properties of microparticles were characterized by scanning electron microscopy (SEM), laser particle size analyzer, x-ray diffractometer (XRD) and differential scanning calorimeter (DSC) respectively. The results indicated that the use of mixed solvent (dichloromethane/acetone) and the polymer concentration played important roles on particle morphology, size and size distribution. In addition the PLLA-PEG-PLLA particles prepared by supercritical antisolvent process have less crystalline.     

HS-LPME-GC法在烟用香精香料质量控制中的应用

采用顶空液相微萃取法(HS-LPME)对8个不同批次及掺兑不同比例其他烟用香精香料的1148#样品的挥发性成分进行提取并用气相色谱法分析,同时研究了不同萃取溶剂、萃取时间、萃取温度对分析结果的影响,确定了最佳条件:样品在70℃下平衡1.0h,搅拌速度300r/min,以4.0μL正十二烷作萃取剂,萃取时间为10min,并通过主成分分析(PCA)法对不同批次及掺兑样品进行模式识别。结果表明:此法能成功地将掺兑样品区分开来,可以成为烟用香精香料1148#质量控制的有效手段之一。     

乙烯基胶原蛋白微球的制备及其应用

为了得到带有“-C=C-”的胶原蛋白微球,我们使用甲基丙烯酸酐对胶原蛋白改性,再采用乳化交联法将改性胶原蛋白制备成乙烯基胶原蛋白微球(CMAs),并将微球应用到尼龙基材上。研究了CMAs的制备条件,使用傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、激光粒度分析仪等对CMAs和乙烯基胶原蛋白微球/尼龙(Nylon-CMAs)进行表征。结果表明,当乙烯基胶原蛋白浓度为15%,转速为800 r/min,交联剂用量为0.8 mL,水油体积比为1∶5,乳化剂用量为2%时,制备的乙烯基胶原蛋白微球的平均粒径为21.204μm,形貌规整、圆整度好,表面光滑,粒径分布较窄。接触角结果显示将微球修饰到尼龙上可以使尼龙由原来的疏水织物变为亲水织物,且制备的织物具有较好的水热稳定性能。     

Preparation and In Vitro/In Vivo Evaluation of Gliclazide Loaded Eudragit Nanoparticles as a Sustained Release Carriers

ABSTRACT

The aim of this study was to formulate and optimize gliclazide-loaded Eudragit nanoparticles (Eudragit L100 and Eudragit RS) as a sustained release carrier with enhanced efficacy. Eudragit L 100 nanoparticles (ELNP) were prepared by controlled precipitation method whereas Eudragit RSPO nanoparticles (ERSNP) were prepared by solvent evaporation method. The influence of various formulation factors (stirring speed, drug:polymer ratio, homogenization, and addition of surfactants) on particle size, drug loading, and encapsulation efficiency were investigated. The developed Eudragit nanoparticles (L100 and RS) showed high drug loading and encapsulation efficiencies with nanosize. Mean particle size altered by changing the drug:polymer ratio and stirring speed. Addition of surfactants showed a promise to increase drug loading, encapsulation efficiency, and decreased particle size of ELNP as well as ERSNP. Dissolution study revealed sustained release of gliclazide from Eudragit L100 as well as Eudragit RSPO NP. SEM study revealed spherical morphology of the developed Eudragit (L100 and RS) NP. FT-IR and DSC studies showed no interaction of gliclazide with polymers. Stability studies revealed that the gliclazide-loaded nanoparticles were stable at the end of 6 months. Developed Eudragit NPs revealed a decreased t_min (ELNP), and enhanced bioavailability and sustained activity (ELNP and ERSNP) and hence superior activity as compared to plain gliclazide in streptozotocin induced diabetic rat model and glucose-loaded diabetic rat model. The developed Eudragit (L100 and RSPO) NP could reduce dose frequency, decrease side effects, and improve patient compliance.     

提高采收率用聚(N-羟甲基丙烯酰胺-丙烯酰胺)微球的反相微乳液聚合及其性能

以煤油为连续相,50.0wt%N-羟甲基丙烯酰胺(N-MAM)、丙烯酰胺(AM)单体水溶液为分散相,Span80/OP-10为乳化剂,依据拟三元相图配制了含50.6wt%油相、42.0wt%水相、7.4wt%Span80/OP-10(质量比6∶1)乳化剂相的W/O微乳液(质量分数)。以N,N-亚甲基双丙烯酰胺(MBAA)为交联剂,在65℃过硫酸铵(APS)引发下进行反相微乳液聚合制备了纳米级交联P(AM/NMAM)微球。以微球粒径及溶胀性为考察指标,从单体配比、交联剂用量、引发剂用量及搅拌速率等方面对合成条件进行了优化。结果表明,在单体配比m(AM)∶m(N-MAM)为4∶1,交联剂MBAA用量0.60wt%、引发剂APS用量0.50wt%(以单体总质量计)、搅拌速率1000r/min的条件下合成的微球耐盐性好、吸水倍率高,在1.0×10~5 mg/L模拟地层水中可达18.40g/g。扫描电子显微镜(SEM)、透射电子显微镜(TEM)对微球形态的表征结果显示,其具有较好的球形度及单分散性,粒径分布均一,约为100nm左右。流变及岩心封堵实验表明微球胶乳具有良好的注入性,封堵效果显著,可实现逐级深部调剖。     

7075铝合金高速搅拌摩擦焊材料流动行为及性能研究

目的 针对7075–O铝合金高焊速、高转速搅拌摩擦焊接缺陷多、质量差等问题,研究焊接接头材料流动对焊缝性能的影响。方法 选用焊接速度1 000 mm/min,搅拌转速分别为1 000、1 200、1 600、1 700 r/min的条件对7075–O铝合金板进行搅拌摩擦焊接,分析不同焊接工艺参数下焊接接头的显微组织及力学性能。同时,利用Fluent软件模拟7075–O铝合金搅拌摩擦焊接过程中的材料流动场分布,分析焊接材料流动与缺陷形成的关系。结果 利用7075–O铝合金三维流动模型,预测出高焊速条件下焊缝前进侧形成一个低压区,孔洞等缺陷易出现在此区域,数值模拟预测与试验结果吻合。在高焊接速度1 000 mm/min、焊接转速1 200 r/min时,焊缝表面光滑平整,焊核区域的硬度分布更加均匀。结论 随着搅拌转速从1 000 r/min增大到1 700 r/min,热输入量逐渐增大,孔洞缺陷由隧道型孔洞转变为不连续的小孔。同时,随着搅拌转速的增大,焊缝高硬度区域的宽度先增大而后降低。当搅拌转速为1 200 r/min时得到了优质的焊接接头,焊缝焊核区硬度分布均匀,硬度值最高为176HV。