American Pharmaceutical Review: A Russell Publishing Publication

New Image Analysis Approach for Particle Size Monitoring of Pharmaceutical Solids

Dr. Niklas Sandler
Senior Researcher, Division of Pharmaceutical Technology
University of Helsinki-Finland

Introduction


If visual or image information is used in science, exact descriptors for this information is usually needed. The utilization of descriptive image information in pharmaceutical powder technology is rather limited. Subsequently, the development of this discipline is a challenge within physical characterization of pharmaceutical solids and process monitoring. In this paper, a new image analysis approach for monitoring of particle size is briefly described. Also, it is shown how the generated image information can be utilized in the prediction of tableting behavior of granules using multivariate methods i.e., chemometrics.


Characterization of Powders - A Key Issue


The characterization of powders and granular materials is of great interest within the pharmaceutical sciences. As approximately 80% of all drug products are solids i.e., tablets or capsules, the understanding of the physical characteristics of powders and granules is essential [1]. For the pharmaceutical industry, a comprehensive knowledge of these materials has a major economic impact. The physical characteristics of solid particulates have to be considered and studied throughout the development process of a product, from the preformulation stage to large-scale manufacturing. In development and manufacturing, many powder handling steps are involved, including crystallization, blending, granulation, and compaction. Thus, different kinds of interactions between particles and between particles and process equipment occur. All these interactions together with specific behavior bulk materials in certain unit operations may give rise to many problems.


Particle Size Measurement of Solids


The bulk properties of a material depend to a great extent on its particle size distribution. Various techniques for measuring the particle size distribution of powders exist. Common methods used with pharmaceutical solids are sieving and laser diffraction. Asingle measurement technique cannot be used to cover the wide size range from nanometers to millimeters. Moreover, many aspects have to be considered before making the proper choice of measurement principle e.g., the capital costs versus running costs, speed of operation, degree of skill required for operation, and most importantly, the end-use requirement. Different particle size analysis techniques are well described in the literature [2]. Most often, microscopy is (has to be) used to verify the particle size measured by “black box” techniques. In order to avoid parallel methodologies, efforts to enhance imaging technologies in particle size have to be made and fortunately, during the recent years, this has happened. In this paper, one approach; a fast particle sizing technique based on surface imaging of undispersed particles, is presented.

When considering classical IAor the measurement of dispersed individual particles. The reluctance of the use of IAin routine analysis of particle morphology e.g., due to relative slowness of the process and the large size of the image as a dataset has been discussed in the literature [3]. Orientation effects of particles can also distort the generated IAdata. Since image processing tasks are needed, the IA procedure is usually performed semiautomatically and a skilled operator is usually needed. The largest source of error in optical IAis probably the sample preparation i.e., the dispersion of the powder. However, automatic sample preparation techniques have been developed lately and automated on-line systems for various processes have also been successfully used over the past decade.


Surface and Bulk Imaging - New Approach


The inspection of surface information can be made in terms of qualitative or quantitative properties. To obtain quantitative information, exact descriptors for the image information are required. In order to receive qualitative data, generalization of the image information is possible. Akey property of a bulk particulate material is a typical pattern of the image field-of-view called “texture” (Figure 1.). Texture is related to distribution of the spatial variation in grey scale levels (or color levels in color images) and can be connected to general bulk-particle characteristics. Global measurements of the texture that are observed in an image can portray information about the size of the particles. Smaller particles lead to finer textures and larger particles to coarser textures. Apparently, the presentation geometry, e.g., the magnification and resolution used, will affect the outcome. Standardized imaging conditions for these kind of textural comparisons are therefore needed. An advantage of textural methods is that particles do not have to be separated from each other and identified individually.

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