Laboratory Equipment and Instruments

Industry and regulatory organizations agree that the current focus on product quality will play a major role in shaping pharmaceutical development in the future. Key to this assessment of quality are the methods and technologies in pharmaceutical analytical testing.

Maintenance and service-related items are often the second-largest budget element in a laboratory after salaries and benefits. Within maintenance, preventive maintenance (PM) is a substantial portion of the budget. Traditionally, PM was an equipment maintenance philosophy based on replacing, overhauling or remanufacturing a piece of equipment at fixed intervals, regardless of its condition at the time. In essence, it involved fixing something that wasn't necessarily broken and this approach is still widely used in the pharmaceutical industry.

High-performance liquid chromatography (HPLC) is a powerful tool for the enantioselective separation of chiral drugs. However, the selection of an appropriate chiral stationary phase (CSP) and suitable operating conditions is a bottleneck in method development and a time- and resource-consuming task. Multimodal screening of a small number of CSPs with broad enantiorecognition abilities has been recognized as the best strategy to achieve rapid and reliable separations of chiral compounds. This paper describes the generic screening strategy developed at Johnson & Johnson Pharmaceutical Research and Development to successfully develop enantioselective HPLC methods for chiral molecules of pharmaceutical interest.

The authors review methods for reducing analysis time and increasing throughput that are reliable and maintain data integrity.

Polysaccharide-based chiral stationary phases have been developed that comprise chiral selectors immobilized on their support rather than being physically coated. These materials are completely solvent stable, thereby increasing selectivity and and enabling the development of new chiral selectors that have been too unstable in a coated form for general use.

Ultrahigh pressure liquid chromatography maximizes efficiency, but, as defined by the resolution equation, the stationary phase is still a crucial consideration when attempting to resolve mixtures of compounds.

A new Raman spectroscopic method to detect magnesium stearate in powder blends and tablets is described. High-volume pharmaceutical manufacturing requires the use of lubricants to facilitate tablet ejection from compressing machines. However, lubricants may also bring a number of undesired problems that have been widely documented in pharmaceutical scientific literature. New analytical methods are needed to understand lubrication and provide process knowledge in support of FDA's process analytical technology initiative. The detection of magnesium stearate in lactose, mannitol, corn starch and other commercially important excipients is reported. The Raman spectroscopic method has a detection limit of about 0.1% (w/w) based on the 2848 cm-1 band that corresponds to the symmetric stretch of the methylene group in magnesium stearate.

Raman spectroscopy has become a commonly used technique for physicochemical analysis that possesses many advantages over other analytical techniques. It is a very attractive characterization tool, not least because it enables measurements in water. However, very few examples of its application in an aqueous environment exist in literature. This paper provides some recent applications of Raman spectroscopy in pharmaceutical material and process characterization when water is present.

This article discusses the advantages and disadvantages of using solid-state NMR spectroscopy for the analysis of pharmaceutical solids.

This article looks at the use of bracketing and matrixing to lower the number of stability samples required and, consequently, reduce the cost of sample production, testing and management. There is a common misconception that regulatory authorities will not accept such methods, but there is actually an International Conference on Harmonization guideline (ICH Q1D) on the subject. In fact, many of these designs have already been accepted and FDA members were among the first to describe matrixing.

The first part of this article introduced the basic features of Raman spectroscopy and presented some examples of its application in the pharmaceutical industry. This second part focusses on the technique's application as a PAT tool within the pharmaceutical manufacturing environment. FDA's PAT initiative has provided motivation to explore the application of 'new' analytical technologies to the pharmaceutical manufacturing process and Raman spectroscopy shows great promise. The strengths and weaknesses of the technique as a potential PAT tool are discussed together with some examples of how this works in practice in a pharmaceutical manufacturing environment.

Detection and identification of different polymorphic forms is, therefore, important throughout the drug development and manufacturing process.

Analytical instrument suppliers are developing manufacturing-tailored tools that are small, precise, and easy to use.

Laser diffraction is an important technique for particle size analysis. This article highlights the many advantages this tool has to offer.

This article describes the quality of highly purified water and its applications, addressing why ultrafiltration (UF) is being used as a downstream purification process. It aims to show that UV is a real alternative for producing pyrogen-free water. This method allows essential cost savings compared with distillation and guarantees a higher safety than other membrane methods such as reverse osmosis.

Rapid structural elucidation of compounds in complex mixtures is a powerful technique in metabolite, degradation and process control applications. The ability to follow the fragmentation pathway through sequential MSn transitions provides added confirmation and increases the selectivity for monitoring compounds of interest in a complex mixture. Previously, the limiting factors in applying this technique were sensitivity at MS4 and higher transitions, and the cycle time required to acquire multiple MSn spectra across a narrow LC peak. Recent developments in trapping, detection efficiencies and scan rates have reduced these limitations and enabled rapid characterization of multiple compounds from single chromatographic runs.

Tosoh has developed a new product - Toyopearl Toyoscreen that allows fast identification of the optimal resin for your sample. You can develop the optimal conditions for the separation in addition to the determination of the dynamic binding capacity. All the resins prepacked in these columns are real process resins concerning particle size. Results on the small columns can be scaled up to production.

Ultrafiltration is a pressure-driven membrane filtering process used to separate and/or purify dissolved or suspended particles from water and other liquids. Recent advances in materials and membrane manufacturing techniques have led to ultrafiltration playing a pivotal role in a number of biopharmaceutical processes, including protein concentration and blood for actionation. This article examines the criteria that should be considered when selecting membranes for such applications.

Measurements of lyophilization pressure are accurate only if the gauges that are used have been properly calibrated.