激光散射法测定苯磺酸氨氯地平原料粒度大小及其分布

建立激光散射法测定苯磺酸氨氯地平原料药粒度大小及其分布的方法.采用Malvern Mastersizer 2000激光粒度分析仪,测定模式干法,样品折射率为1.55、吸收率为0.10,遮光度0.5％～5.0％,仪器设置参数为样品测量时间5 s、气源压力1.0 bar、进样速度60％、狭缝宽度0.5 cm.优化后的方法验...     

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。     

纳米雄黄的粒度分析方法

目的：建立纳米雄黄的粒度分析方法。方法：利用原子力显微镜对纳米雄黄的表观形貌进行直接观察测定,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：首次得到原子力显微镜下纳米雄黄形貌特征图;激光光散射颗粒度测定仪的测量显示．粒径在30nm以下的纳米雄黄约90％。结论：本研究所采用的原子力显微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。     

激光衍射法测定对乙酰氨基酚粒度分布的方法研究

目的 利用激光衍射法建立对乙酰氨基酚粒度与粒度分布的测定方法。方法 采用马尔文Mastersizer 2000激光粒度分析仪,湿法测定对乙酰氨基酚的粒度与粒度分布。样品采用含0.1%大豆卵磷脂的正己烷溶液,样品折射率1.70,样品吸收率0.1,遮光度范围10%～20%,超声20 s,泵转速2 000 r·min^–1。结果 激光衍射法可以测定对乙酰氨基酚的粒度及其分布,由体积平均粒径D[4,3]可以直观表征对乙酰氨基酚粒度的大小差异。d(0.5)值的RSD<3%,d(0.1)和d(0.9)值的RSD均<5%,方法重复性较好。结论 本法快速、简便、重复性好,可用于对乙酰氨基酚粒度及粒度分布的测定。     

激光散射法测定羧甲纤维素钙粒度与粒度分布的研究

目的 建立激光散射法测定羧甲纤维素钙的粒度与粒度分布.方法 采用Malvern Mastersizer 2000型激光散射粒度分析仪,干法测定模式,样品折射率1.52,颗粒吸收率0.1,分散介质折射率1.00,空气分散压力0.5 bar,振动进样速度40％,测量时间10 s,进样口宽度7 mm,遮光度0.5％～5％.结...     

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。     

光散射法测定难溶性药物粒度

目的 研究光散射法中湿法测定难溶性药物粒度的方法及要求.方法 HT6K 通过仪器参数设定、样品的制备、分析方法验证确定原料药粒度测定的方法,根据生产工艺、体外溶出及体内吸收制定原料药粒度标准,对利伐沙班原料药进行粒度测定.结果与结论 粒度对药物的有效性、安全性、稳定性都有重要影响,湿法测定原料药的粒度方法稳定、结果准确、重现性好,在药物开发过程中应对药物粒度的测定方法进行详细研究并制定符合要求的粒度标准.     

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。     

激光散射法测定布洛芬混悬液粒度的研究

目的 建立激光散射法测定布洛芬混悬液中布洛芬的粒度及粒度分布的方法。方法 使用Malvern Mastersizer 2000激光粒度分析仪,Hydro 2000SM进样器;背景及样品的扫描时间为15 s,搅拌速率为850 r/min;分散剂为水,以辅料溶液为背景测试样品溶液;颗粒折射率为1.400～1.500;颗粒的吸收率为0.001;遮光度为5%～20%。结果 激光散射法可以测定布洛芬混悬液的粒度及其分布,由体积平均粒径D(4,3)可以直观地表征不同批号的布洛芬混悬液中布洛芬颗粒的大小差异,由d(0.1)、d(0.5)、d(0.9)数值表示其粒度分布的特征。方法学考察结果和样品测定结果的d(0.1)、d(0.5)和d(0.9)的RSD均小于8%。结论 本方法适合布洛芬混悬液中布洛芬药物的粒度及粒度分布的测定。     

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。     

微乳型丙泊酚纳米注射液的制备与评价

目的:制备微乳型丙泊酚纳米注射液,并对其进行体内外评价,为新型微乳型纳米注射液研究提供参考。方法:使用可注射用乳化剂和油制备丙泊酚纳米注射液,旋转黏度计测定其黏度,动态光散射法测定其粒径和Zeta电位,透射电镜测定其显微外观,透析法测定其游离药物浓度,并研究其体外溶血性和Beagle犬体内药动学性质。结果:黏度为1.5×10-3 Pa.s,粒径为(22.7±10.2)nm,Zeta电位为-5.82 mV;透射电镜照片显示微乳粒子外观近球状,游离药物浓度为(17.9±0.8)μg.mL-1(n=3),不引起溶血的发生;微乳与脂肪乳主要药动学参数t1/2α分别为(1.506±0.994)和(2.512±2.122)min,t1/2β分别为(42.221±43.878)和(49.095±42.521)min,V1分别为(1.947±1.17)和(3.546±3.836)L.kg-1,CL分别为(0.218±0.07)和(0.219±0.068)L.min-1.kg-1,AUC0～t分别为(17.916±6.772)和(16.968±5.395)mg.min.L-1,AUC0～∞分别为(20.488±7.729)和(...     

Particle size determination using the method of dynamic light scattering

Realising the lacks of the classic methods of particle size determination a new method was needed to be developed which became suitable for measurements in the nano range as well. The principle of this method was discovered more than 20 years ago but manufacturers are still able to insert novelties by developing and refining the technique of - dynamic light scattering. Importance of multiparticular systems increases in pharmaceutical technology. It is necessary to apply this new method to investigate them.     

Critical Evaluation of Microfluidic Resistive Pulse Sensing for Quantification and Sizing of Nanometer- and Micrometer-Sized Particles in Biopharmaceutical Products

The objective was to evaluate performance, strengths, and limitations of the microfluidic resistive pulse sensing (MRPS) technique for the characterization of particles in the size range from about 50 to 2000 nm. MRPS, resonant mass measurement (RMM), nanoparticle tracking analysis (NTA) and dynamic light scattering were compared for the analysis of nanometer-sized polystyrene (PS) beads, liposomes, bacteria, and protein aggregates. An electrical conductivity of at least 3 mS/cm (equivalent to 25 mM NaCl) was determined as a key requirement for reliable analysis with MRPS. Particle size distributions of PS beads determined by MRPS, NTA, and RMM correlated well. However, counting precision varied significantly among the techniques and was best for RMM followed by MRPS and NTA. As determined by measuring single and mixed PS bead populations, MRPS showed the highest peak resolution for sizing. RMM and MRPS were superior over dynamic light scattering and NTA for the characterization of stressed protein samples. Finally, MRPS proved to be the only analytical technique able to characterize both bacteria and liposomes. In conclusion, MRPS is an orthogonal technique alongside other established techniques for a comprehensive analysis of a samples particle size distribution and particle concentration.     

Investigation of Pharmaceutical Oil/Water Microemulsions by Small-Angle Scattering

Purpose. Stable oil/water (o/w) microemulsions are very effective vehicle systems for dermal administration of drugs having no or low skin penetration. These systems, consisting of oils, a blend of a high and a low HLB surfactant, and a hydrophilic phase (propylene glycol/water), were developed using pharmaceutically acceptable components. Methods. In this paper, the droplet size of these microemulsions was characterized by means of dynamic light scattering (DLS) and small-angle neutron scattering (SANS). Furthermore, different size parameters obtained by DLS and SANS experiments were compared and discussed. Results. Extremely small droplet radii of approximately 10 nm could be observed. A good agreement between the data of DLS and SANS experiments was found. The kind of oil only marginally influences the droplet size. Conclusions. Particle size determination via scattering techniques is a useful tool to characterize droplets in microemulsions for dermal drug delivery.     

Microviscosity and drug release from topical gel formulations

Gel formulations are often used in topical drug delivery, and the drug release is controlled by two factors, the thermodynamic activity of the drug and the microviscosity of the gel. The latter property has been probed by observing the dynamic light scattering from polystyrene lattices of known particle size dispersed within Carbopol gels. The effect of gel concentration and temperature has been observed and related to the ability of the gel to release a series of salicylates.     

Insulin aggregation in solution

The process of insulin aggregation in neutral solutions was studied by dynamic light scattering. Solutions of different concentrations were subjected to thermal and mechanical stress (37°, rotation) for a period of 4 weeks. The starting solutions contained exclusively one particle distribution of insulin in the association equilibrium with hexamers as the largest structures. After a lag period of about 8 days the solutions showed continuously increasing scattering intensities but did not evolve perceptible turbidity within the experimental period. A more rapid increase in scattering intensity was observed in diluted than in concentrated solutions. The analysis of scattering data unexpectedly revealed that insulin species did not grow continuously. After the lag period one additional relatively restricted size distribution with particles of a mean radius of about 100nm was found, the amount of which increased continuously with time. The occurrence of these particles seems to be related to adsorption phenomena of insulin to the solid interface. We assume the 100nm-class of aggregates to be a transient state in the physical destabilization process of insulin solutions.     

激光粒度仪测定单硝酸异山梨酯缓释片中间产品粒度的方法学研究

目的 建立测定单硝酸异山梨酯缓释片中间产品粒度分布的方法。方法 采用Malvern Mastersizer 3000型激光粒度分析仪,Aero S型干法进样器。激光散射法干法检测参数为：样品折射率1.52、漏斗池高度1.0 mm、遮光度范围0.8%～3.0%、分散气体压力2.0 bar、进样速度50%、样品测量时间25 s。结果 同一批供试品,平行测定6次,不同操作人员在不同时间、使用相同仪器和相同方法,测得粒度分布结果的RSD值小于1.0%;三个批次供试品,相同操作人员使用相同仪器和相同方法测得批次间粒度分布结果的RSD值小于2.0%。结论 该方法重现性好、准确度高,操作简便,可用于单硝酸异山梨酯缓释片中间产品粒度分析。     

Characterization of nanomaterial dispersion in solution prior to in vitro exposure using dynamic light scattering technique.

The need to characterize nanoparticles in solution before assessing the in vitro toxicity is a high priority. Particle size, size distribution, particle morphology, particle composition, surface area, surface chemistry, and particle reactivity in solution are important factors which need to be defined to accurately assess nanoparticle toxicity. Currently, there are no well-defined techniques for characterization of wet nanomaterials in aqueous or biological solutions. Previously reported nanoparticle characterization techniques in aqueous or biological solutions have consisted of the use of ultra-high illumination light microscopy and disc centrifuge sedimentation; however, these techniques are limited by the measurement size range. The current study focuses on characterizing a wide range of nanomaterials using dynamic light scattering (DLS) and transmission electron microscopy, including metals, metal oxides, and carbon-based materials, in water and cell culture media, with and without serum. Cell viability and cell morphology studies were conducted in conjunction with DLS experiments to evaluate toxicological effects from observed agglomeration changes in the presence or absence of serum in cell culture media. Observations of material-specific surface properties were also recorded. It was also necessary to characterize the impact of sonication, which is implemented to aid in particle dispersion and solution mixture. Additionally, a stock solution of nanomaterials used for toxicology studies was analyzed for changes in agglomeration and zeta potential of the material over time. In summary, our results demonstrate that many metal and metal oxide nanomaterials agglomerate in solution and that depending upon the solution particle agglomeration is either agitated or mitigated. Corresponding toxicity data revealed that the addition of serum to cell culture media can, in some cases, have a significant effect on particle toxicity possibly due to changes in agglomeration or surface chemistry. It was also observed that sonication slightly reduces agglomeration and has minimal effect on particle surface charge. Finally, the stock solution experienced significant changes in particle agglomeration and surface charge over time.     

激光散射法测定阿维A原料药粒度

目的：建立测定阿维A原料药的粒度及其分布的方法。方法：采用Malvern Mastersizer2000激光粒度分析仪、Hydro 2000MU湿法进样器,以《中国药典》粒度和粒度分布测定法中的光散射法进行阿维A原料药的粒度分析并进行方法学考察,泵速为1500r/min,遮光比为5%～15%,背景与样品的扫描时间为5s,样品折射率为1.569,样品吸光率为0.01。结果：方法学考察结果d（0.5）的RSD均〈3%,d（0.1）和d（0.9）的RSD均〈5%;4批阿维A原料药的d（0.1）均小于5μm,d（0.5）均小于10μm,d（0.9）均小于20μm,符合《中国药典》相关要求。结论：该方法简便、准确、重复性好,适用于阿维A原料药的粒度控制。     

研究蒙脱石原料及其散剂的粒度与晶体杂质

目的:建立更为有效的激光粒度法与X-射线衍射法测定国产蒙脱石原料及其散剂的粒度与晶体杂质。方法:粒度测定:使用马尔文2000激光粒度仪,在800 mL水中以3000 r·min-1搅拌15 min,湿法测定。晶体杂质测定:采用X-射线衍射法;阴极:铜;滤过片:镍;电源:45 kV、40 mA;狭缝:0.1°;衍射角(2θ)从2°到80°扫描。结果:考察的5个企业15批蒙脱石原料中,60%均检出致癌物方英石;生产蒙脱石散的20个企业样品65%的产品检出方英石。结论:激光粒度法更为真实地反映了蒙脱石粒度的分布情况,可明显区分不同企业蒙脱石粒度的差别。X-射线衍射法可有效控制蒙脱石及其散剂中致癌物方英石的量。