Determination of the particle size of realgar nano-particles by scanning 

目的：建立纳米雄黄的粒度分析研究方法。方法：利用扫描电镜对纳米雄黄表观形态进行直接观察测定,用激光光散射法对纳米雄黄的粒度分布范围进行分析测定。结果：经扫描电镜和激光光散射颗粒度测定仪的测量,粒径在100 nm以下的纳米雄黄约达90%,其中较大颗粒又是由粒径在5~30 nm左右的细小晶粒和其周围的非晶体聚集而成。结论：扫描电镜法和激光光散射法快速、简便、准确,可用于纳米雄黄的粒度检测。     

纯化纳米雄黄制备方法探讨

目的探讨纯化纳米雄黄的制备方法,以制备高纯度、高生物利用度、低毒副作用的纯化纳米雄黄颗粒。方法①天然雄黄经去离子水和不同浓度的HCl、NaOH纯化处理后得到纯化雄黄,测定As2S2含量;②天然雄黄、纯化雄黄经高能球磨法制备得到天然纳米雄黄、纯化纳米雄黄,颗粒经扫描电镜、纳米粒度分析仪测定纳米颗粒形貌、粒径,测定As2S2含量;③天然纳米雄黄、纯化纳米雄黄经2.0 mol·L-1的HCl纯化处理得到天然纳米雄黄(纯化组)、纯化纳米雄黄(纯化组),扫描电镜、纳米粒度分析仪测定纳米颗粒形貌、粒径;测定As2S2含量。结果①去离子水;0.5、1.0、2.0、4.0 mol·L-1的HCl与NaOH纯化处理后颗粒As2S2含量均有所提高,各处理组之间差异有统计学意义(P<0.05);纯化效果:HCl组>NaOH组>去离子水组,随着HCl、NaOH浓度的提高,As2S2的含量亦随之提高;以4.0 mol·L-1 HCl组纯化效果最显著,其次为2.0 mol·L-1HCl组。②天然雄黄、纯化雄黄、天然纳米雄黄(纯化组)、纯化纳米雄黄(纯化组)经高能球磨法可制备得到纳米级雄黄颗粒,扫描电镜可见近似圆球形的纳米级颗粒,粒度分布均匀,纳米粒度分析仪测定其平均粒度分别为(135.13±9.19)、(134.39±4.57)、(135.88±2.68)、(133.73±4.36)nm;As2S2含量分别为(92.09±0.83)%、(97.07±0.47)%、(97.42±0.11)%、(98.33±0.08)%。纳米雄黄组与纳米雄黄(纯化组)粒度差异无统计学意义(P>0.05),纯度差异有统计学意义(P<0.05)。结论①去离子水、HCl、NaOH均可对雄黄进行纯化处理,以HCl纯化效果为最好;②高能球磨法可制备纳米雄黄颗粒;③球磨前后分别对雄黄颗粒进行纯化处理,可得到As2S2含量更高的纯化纳米雄黄颗粒。     

两性霉素B脂质体粒度测定方法研究

目的：建立两性霉素B脂质体粒度检测方法，通过测定一组性质不同的样品，找出最佳测定方法。方法：用计算机的图像一数字处理技术结合扫描电镜、透射电镜和激光光散射粒度测定仪分别测定两性霉素B脂质体的粒度。结果：电镜法测定两性霉素B脂质体的粒度为20—100nln，平均粒径为55—75nm；激光光散射法测定两性霉素B脂质体的粒度为30—200nm，平均粒径为50—180nm。结论：激光光散射法能较好反映两性霉素B脂质体在使用时的真实粒度，且方法快速、简便，是一种较好的两性霉素B脂质体粒度测定方法。     

丙泊酚注射液乳粒粒径测定方法探讨

目的：对乳粒粒径测定的方法及仪器参数的设置进行初步探讨。方法：采用经典光散射法,使用马尔文激光散射粒度测定仪分别对仪器的3个参数（遮光度、吸收率、折射率）的设置范围进行考察;以丙泊酚注射液为模型药物,用动态光散射法与经典光散射法测定相同的13批样品,比较平均粒径及小于0．4pm粒子的百分比这2项指标测定结果的差异。结果：马尔文公司的激光粒度测定仪参数设置范围为遮光度5％～10％、吸收率0～0．01、折射率1．47～1．52时对粒径测定结果影响不大;与经典光散射法测得的结果比较,动态光散射法测得的平均粒径较小,测得的小于0．4um的粒子的百分比更大;确立丙泊酚注射液乳粒测定方法为经典光散射法。结论：本试验建立的粒径测定方法及仪器参数可用于不同厂家丙泊酚注射液的粒径测定,使各厂家产品质量具有可比性;本方法的建立为其他类似品种注射剂的粒径测定提供了研究方向及恩路。     

两性霉素B脂质体粒度测定方法研究

目的建立两性霉素B脂质体粒度检测方法,通过测定一组性质不同的样品,找出最佳测定方法。方法用计算机的图像-数字处理技术结合扫描电镜、透射电镜和激光光散射粒度测定仪分别测定两性霉素B脂质体的粒度。结果电镜法测定两性霉素B脂质体的粒度为20～100nm,平均粒径为55～75nm;激光光散射法测定两性霉素B脂质体的粒度为30～200nm,平均粒径为50～180nm。结论激光光散射法能较好反映两性霉素B脂质体在使用时的真实粒度,且方法快速、简便是一种较好的两性霉素B脂质体粒度测定方法。     

在不同温度条件下用戊二醛交联制备聚乙烯亚胺的纳米结构

研究了在不同温度下(30℃,50℃,65℃)聚乙烯亚胺与戊二醛的交联反应,并对产生的各种纳米结构进行了表征.目的是为了制备聚乙烯亚胺的各种纳米结构,为进一步开发聚乙烯亚胺作为药物载体进行探索.对交联反应产物的结构和形貌,表面电位和光谱性质运用原子力显微镜,激光粒度仪和紫外分光光度计进行了表征.结果表明不同温度条件下反应...     

纳米雄黄抗B细胞非霍奇金淋巴瘤Raji细胞的体外作用研究

目的考察纳米雄黄对B细胞非霍奇金淋巴瘤Raji细胞的体外作用。方法利用激光粒度仪、TEM和AFM对纳米雄黄和水飞雄黄进行表征;利用光镜、AFM和TEM依次观察纳米雄黄和水飞雄黄作用下Raji细胞的增殖形态变化、单细胞表面细胞膜变化以及细胞内超微结构的变化;MTT法检测纳米雄黄和水飞雄黄作用下的细胞存活率;利用荧光显微镜及流式细胞术观察纳米雄黄和水飞雄黄引起Raji细胞的凋亡和细胞周期分布情况。结果纳米雄黄的粒径为(79±8)nm,水飞雄黄的粒径为(1.89±0.2)μm。光镜下,可明显观察到纳米雄黄可抑制Raji细胞的聚集生长状态,AFM下可观察到纳米雄黄作用下的Raji细胞皱缩,体积变小,膜表面的黏附物质不再向四周伸展,而水飞雄黄作用下的Raji细胞变化不明显。TEM下可观察到纳米雄黄作用下的Raji细胞胞内亚细胞器受到破坏,线粒体空泡明显增多,水飞雄黄组变化不明显。MTT结果显示,50 mg·L~(-1)纳米雄黄作用Raji细胞24 h时,细胞的存活率为(40±2)%,而相同剂量的水飞雄黄作用组为(65±3)%;50 mg·L~(-1)纳米雄黄作用Raji细胞48 h时,Raji细胞的存活率仅为10%,而相同剂量的水飞雄黄组,Raji细胞的存活率为(42±2)%。荧光显微镜下可观察到纳米雄黄作用下的Raji细胞核凋亡明显,水飞雄黄组作用不明显。流式细胞术结果显示,水飞雄黄作用下的Raji细胞总凋亡率为11.14%,而纳米雄黄处理组的Raji细胞总凋亡率为15.9%。与水飞雄黄相比,纳米雄黄作用下Raji细胞在G_1期的分布比例明显升高,S期分布比率下降。结论与水飞雄黄相比,相同剂量的纳米雄黄在相同作用时间下,可明显抑制B细胞淋巴瘤Raji细胞的增殖,破坏其亚细胞结构,进而引起其凋亡。     

激光散射法测定乳糖的粒度

目的：确定激光散射法测定乳糖粒度分布，并与传统的筛分法进行比较。方法：Malvem Mastersizer 2000激光粒度分析仪，Scirocco 2000干法进样器；振动进样速度为50％；分散气压，60目和200目为2×10^5Pa，70目、80目、100目为5×10^4Pa；背景及样品的扫描时间为15s；遮光度为0．5％～5％；颗粒折射率为1．347；颗粒吸收率为0．1。Sympatec Helos＆Rodos激光粒度分析仪，振动进样速度为60％；分散气压为5×10^4Pa；透镜为2．5mm，遮光度为4％～10％。OCTAGON DIGITAL高速筛分机；筛分时间2min；振动幅度9。结果：激光散射法可以测定各种规格的乳糖样品，由体积平均粒径D[4，3]可以直观地表征不同规格的乳糖颗粒大小的差异，由d（0．1）、d（0．5）和d（0．9）可以看出其粒度分布特征。基于米氏理论或弗朗霍夫理论进行运算的激光粒度仪均可用于乳糖的粒度分析，两者的测定结果无显著性差异。结论：虽然筛分法与激光散射法均可以表征乳糖的粒度分布，但激光散射法能更好地表征样品的粒度分布，同时可减少测量过程中人为操作误差的影响。     

磁性吉西他滨隐形纳米脂质体的制备及其理化性质

目的:研究制备磁性吉西他滨隐形纳米脂质体(MGSL)的最佳条件.并对其质量进行检测.方法:通过逆相蒸发法制备MGSL,采用扫描电镜和原子力显微镜时其形态进行观察;利用激光粒度分析仪测定MGSL粒径大小和粒度分布;通过高效液相色谱法检测药物的栽药量和包封率;使用专业磁性测试仪进行体外磁响应性测定,且对MGSL的稳定性进行评价.结果:MGSL为圆形或椭圆形,大小均匀一致,其平均粒径为206.6 nm,粒度分布窄,大小均匀.MGSL载药量为(10.4±0.7)%,包封率为(81.7±5.1)%.并具有体外磁响应性好、稳定性高等特点.结论:本法制备的MGSL符合纳米磁靶向给药系统的条件,有望成为一种有效的抗肿瘤物质.     

载多柔比星PEG-PLGA纳米胶束制备及其抗三阴性乳腺癌作用

目的制备载多柔比星(Dox)聚乙二醇-聚乳酸聚乙醇酸(PEG-PLGA)纳米胶束,并研究其抗三阴性乳腺癌作用。方法以D,L-丙交酯和乙交酯为原料,采用本体聚合法合成PEG-PLGA共聚物,通过透析法制备Dox-PEG-PLGA纳米胶束;核磁共振1HNMR对其结构进行表征;透射电子显微镜观察纳米粒形态;激光粒度仪测定平均粒径、粒径分布;紫外分光度法测定纳米粒的载药率、包封率及体外释放;MTT法评价Dox-PEG-PLGA对鼠TNBC细胞4T1的细胞毒性,并通过流式细胞术和激光共聚焦显微镜检测药物内吞。结果制备的纳米胶束呈圆形,大小较为均一,平均粒径约为135 nm,载药率为(9.70±0.33)%,包封率为(71.63±1.33)%;且工艺重现性良好,在96 h下呈现缓慢释放。Dox和Dox-PEGPLGA 24 h半数抑制浓度(IC50)分别为2.355 428和14.446 3μg·mL~(-1)。结论 Dox-PEG-PLGA纳米胶束具有较小的粒径、良好的缓释性能并能显著提高抗肿瘤效能。     

Preparation of nanocapsules containing the two-phase core materials

In this study, copolymer nanocapsules containing the two-phase core materials were prepared by mini-emulsion polymerization using styrene (St) and methylmethacrylate (MMA) as comonomer, in which the ZnO nanoparticles organic suspension was prepared by solvothermal synthesis method. The obtained materials were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), UV-visible spectrophotometry and fluorescence spectrometer. The particle size of the prepared ZnO nanoparticles dispersed in the organic solvent was less than 20 nm. The resulting polymer nanocapsules have 100-200 nm in diameter and approximately 10-20 nm in the wall thickness. The surface of the polymer nanocapsules is smooth and clear.     

Preparation of nanocapsules containing the two-phase core materials

In this study, copolymer nanocapsules containing the two-phase core materials were prepared by mini-emulsion polymerization using styrene (St) and methylmethacrylate (MMA) as comonomer, in which the ZnO nanoparticles organic suspension was prepared by solvothermal synthesis method. The obtained materials were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), UV-visible spectrophotometry and fluorescence spectrometer. The particle size of the prepared ZnO nanoparticles dispersed in the organic solvent was less than 20?nm. The resulting polymer nanocapsules have 100–200?nm in diameter and?～?10–20?nm in the wall thickness. The surface of the polymer nanocapsules is smooth and clear.     

Characterization of Crystalline Drug Nanoparticles Using Atomic Force Microscopy and Complementary Techniques

Purpose. The purpose of this work was to image crystalline drug nanoparticles from a liquid dispersion and in a solid dosage form for the determination of size, shape, and distribution. Methods. Crystalline drug nanoparticles were adsorbed from a colloidal dispersion on glass for atomic force microscopy (AFM) imaging. Nanoparticles that were spray coated onto a host bead were exposed by ultramicrotomy for scanning electron microscopy and AFM examination. Results. The adsorbed drug nanoparticles were measured by AFM to have a mean diameter of 95 nm and an average aspect ratio of 1.3. Nanoparticles observed in the solid dosage form had a size and shape similar to drug nanoparticles in the dispersion. Particle size distribution from AFM measurement agreed well with data from field emission scanning electron microscopy, static light scattering, and X-ray powder diffraction. Conclusions. AFM is demonstrated to be a valuable tool in visualization and quantification of drug nanoparticle crystals in formulations. In addition to accurate size measurement, AFM readily provides shape and structural information of nanoparticles, which cannot be obtained by light scattering. Ultramicrotomy is a good sample preparation method to expose the interior of solid dosage forms with minimal structural alteration for microscopic examination.     

汉黄芩素固体脂质纳米粒的制备及体外释放度考察

目的:制备汉黄芩素固体脂质纳米粒并对其体外释放度进行考察.方法:采用乳化分散-超声法制备汉黄芩素固体脂质纳米粒,以包封率和载药量为评价指标,进行正交试验筛选最优处方,并对最优处方的外观、粒径和体外释放度进行考察.结果:制得的纳米粒为均一球形,平均粒径为(153 ±34)nm,其平均载药量为(60.53±2.17)％,平均包封率为(85.54±4.16)％,48 h累积释放达80％.结论:本试验获得了较理想的汉黄芩素固体脂质纳米粒,其体外释放具有缓释作用.     

载ACE-shRNA pGenesil质粒与壳聚糖纳米粒的结合及释放实验

目的制备适当粒径的壳聚糖纳米粒,并连接上质粒,研究壳聚糖纳米粒对质粒DNA的结合能力及在体外的释放。方法采用离子交联法制备壳聚糖纳米粒,通过喷金电镜观察其大小、形态及分布;经琼脂糖凝胶电泳分析纳米载体与质粒DNA的结合能力;在4种不同pH值的磷酸盐缓冲液(PBS)中观察壳聚糖质粒纳米粒的释放情况;通过紫外分光光度计检测其包埋率及释放率。结果喷金电镜证实壳聚糖纳米粒分布均匀,呈近似球形,平均粒径约5nm;琼脂糖凝胶电泳结果显示壳聚糖纳米粒能有效地结合质粒,当纳米粒与质粒的比例为10∶10时包埋率达98.7%;壳聚糖质粒纳米粒的性质较稳定,在pH值<7.5的PBS溶液能够平稳释放100h左右。结论制备出适当粒径且分布均匀的壳聚糖纳米粒,能有效地结合质粒,并且能够持续平稳地释放。     

大鼠口服雄黄后砷的药物动力学与毒代动力学研究

目的：探讨大鼠口服不同剂量雄黄后砷的药动学及毒代动力学规律。方法：氢化物发生．原子荧光光谱法测定大鼠单次灌胃3．5g·kg^-1和7．0g·kg^-1。雄黄后不同时间的血及组织中砷含量,拟合药动学模型,计算药动学参数。结果：大鼠单次口服雄黄后砷的药动学特征符合一室模型,3．5g·kg^-1和7．0g·kg^-1两个剂量组主要药动学和毒代动力学参数分别为：t1／2：15．87h和16．87h;Cmax：3．74×10^2μg·L^-1和6．89×10^2μg·L^-1;AUC0—6：9．86×10^3μg·h·L^-1和1．69×10^4μg·h·L^-1。砷在各组织均有分布,以肝、肾中含量最高。结论：大鼠口服不同剂量雄黄后砷在大鼠血中的药动学过程基本一致,在体内可造成蓄积。     

Purification and aqueous phase atomic force microscopic observation of recombinant P2X2 receptor

Recombinant P2X2 receptor was observed by atomic force microscope in the aqueous phase. The P2X2 receptor was expressed in an insect cell line, and recombinant proteins were prepared under native conditions. The membrane fractions were extracted, and histidine-tagged receptor protein was purified from the fractions by column chromatography. When the purified protein fraction was diluted with water and served for atomic force microscopy, dispersed particles of about 3 nm in height were observed. In the presence of 1 mM ATP, the assembly-like images of the particles were obtained. More densely assembled images of the particles were achieved when the protein was dissolved in a Tris buffer containing 1 mM ATP. Under this condition, imaging of the surface of the particles exhibited a circular structure with a diameter of about 10 nm having a pore-like structure. These results suggest that atomic force microscopy provides structural information about P2X2 receptor in aqueous phase.     

Preparation, characterization and protein loading of hexanoyl-modified chitosan nanoparticles

Hexanoyl chitosan was synthesized through a coupling reaction between chitosan and hexanoic anhydride. Proton nuclear magnetic resonance (¹HNMR) and fourier-transform infrared (FTIR) spectroscopy studies showed the formation of hexanoyl chitosan. The nanoparticles of hexanoyl chitosan were prepared through ionotropic gelation with tripolyphosphate (TPP) followed by sonication. The hexanoyl chitosan-TPP nanoparticles exhibited uniform spherical shape with smooth surface as observed by atomic force microscopy and transmission electron microscopy. The particle size of nanoparticles was between 54.1 to 724 nm with a mean diameter of 324 nm. At 0.2, 0.4, and 0.6 mg/mL bovine serum albumin initial concentration, the encapsulation efficiency and loading capacity of hexanoyl-chitosan-TPP nanoparticles were 58.2, 44.5, and 28.1%, and 14.1, 23.4, and 30.3%, respectively.