Equipment, analytical suppliers

Surface and Thin Film Analytical Equipment Suppliers... 

Many companies now supply surface and thin film analytical equipment although a few provide several techniques, most specialize in just one or two. (Only suppliers of the equipment which is discussed in more detail are given in the list helow. The authors cannot guarantee completeness.)... 

Finally, the recording of many signals from the output of the analytic and electrochemical instrumentation requires a reliable multi-pen recorder or an equivalent recording system based on a data acquisition card and appropriate software. The recorded signals are normally in the range of a few mV to 10V. The use of reliable temperature controllers and thermocouples is also crucial for the success of the experiments. A lot of suppliers of such equipment can be easily found and will not be reported here. 

Distributors of general laboratory equipment also offer one or more lines of work benches and fume hoods, often shown in a separate catalog. In addition, there are several companies specializing in this field. The annual LabGuide issue of Analytical Chemistry, published by the American Chemical Society, has a good listing of suppliers. A laboratory planner should obtain catalogs from several sources and compare both features and prices. 

DQ is performed by the supplier of the equipment or system at the supplier s factory as part of the factory acceptance test (FAT). IQ (based on site acceptance test—SAT), OQ, and PQ are performed on-site at the GMP facility. For a GMP manufacturing facility, the validation activities include the facility design, FTVAC system, environment control, laboratory and production equipment, water system, gases and utilities, cleaning, and analytical methods. Validation protocols (IQ, QQ, and PQ) are prepared for each item, listing all critical steps and acceptance criteria. Deviations are reviewed and resolved before the validation activity proceeds to the next phase. 

On-line size exclusion chromatographic (SEC) analyses were performed with a Waters Model 401 differential refractometer (DR), a Waters Model 480 ultraviolet (UV) variable wavelength spectrophotometer and a Foxboro Miran lA infrared (IR) photometer, equipped with a zinc selenide ultramicro flowcell of 1.5 mm nominal pathlength and 4.5 /xl volume, purchased from the same supplier. A set of ten Mycrostyra-gel (Waters Associates) columns, regenerated by Analytical Sciences Inc. (ASI) and of nominal porosities 100, 500 (two) 10 (two), 10 (three), 10 and lO X, in the order given and a mobile phase flow rate of 1 ml/min was used. The column set had a specific resolution of 19.7 in 1,4-dioxane, as determined by the method of Yau(2). 

Analytical Development. The increasingly complex molecules require a permanent development of new, sophisticated analytical methods and, if required, their validation. In order to fulfill this demanding task, a well-equipped state-of-the-art analytical laboratory has to be accessible. In custom manufacturing projects, a close cooperation between the analytical departments of the customer and the supplier is essential for a successful completion of a project. 

The information in this chapter applies specifically to the first element sample preparation. The sample preparation steps are usually the most tedious and labor-intensive part of an analysis. By automating the sample preparation, a significant improvement in efficiency can be achieved. It is important to make sure that (1) suitable instrument qualification has been concluded successfully before initiation of automated sample preparation validation [2], (2) the operational reliability of the automated workstation is acceptable, (3) the analyte measurement procedure has been optimized (e.g., LC run conditions), and (4) appropriate training in use of the instrument has been provided to the operator(s). The equipment used to perform automated sample preparation can be purchased as off-the-shelf units that are precustomized, or it can be built by the laboratory in conjunction with a vendor (custom-designed system). Off-the-shelf workstations for fully automated dissolution testing, automated assay, and content uniformity testing are available from a variety of suppliers, such as Zymark (www.zymark.com) and Sotax (www.sotax.com). These workstations are very well represented in the pharmaceutical industry and are all based on the same functional requirements and basic principles. 

The adsorbent slurry may be applied to the TLC plates by means of several methods. For analytical work, the plates are best prepared with a special TLC adsorbent applicator which provides uniform layers and can be often adjusted to various thicknesses from 250 pm (normal) up to 500 or 1000 pm for preparative separations. The preparation of plates with a typical applicator is shown in Fig.3.1. These applicators are available from a number of suppliers of TLC equipment including most of those mentioned in Table 3.2. After the slurry has been applied, the plates are dried in air overnight or in a warm oven at 80-90°C for ca. 30 min. The dry plates are stored in a dust-free cupboard for further use. Portable cabinets for plate storage are available from a number of suppliers. 

Most of the routine TLC equipment mentioned above can be obtained from the major suppliers listed in Tables 3.1 and 3.2. These items and accessories are available in many styles, shapes and sizes, and are suitable for most analytical requirements. 

Scope of Validation The boundaries of the validation project must be defined to ensure that there is full coverage. For example, will the analytical equipment or Chromatography Data System interfaces be validated as part of the project, will Supplier Evaluations be required, etc. It is very important at this stage to determine what is within the scope of the LIMS Validation Plan and what will be validated under other associated Validation Plans. The validation of the implementation of processes and information management within the laboratory should be managed as a cohesive whole to ensure that all parts of the LIMS are developed and validated to the appropriate standards. This may be achieved by the use of a Validation Master Plan (VMP) for all the laboratory processes and information management. The Validation Plan for the LIMS and any associated plans for other interfaced systems would be referenced in and be under the control of this VMP. 

Reproducibility, as defined by ICH, represents the precision obtained between laboratories with the objective of verifying if the method will provide the same results in different laboratories. The reproducibility of an analytical method is determined by analyzing aliquots from homogeneous lots in different laboratories with different analysts, and by using operational and environmental conditions that may differ from, but are still within the specified, parameters of the method (interlaboratory tests). Various parameters affect reproducibility. These include differences in room environment (temperature and humidity), operators with different experience, equipment with different characteristics (e.g., delay volume of an HPLC system), variations in material and instrument conditions (e.g., in HPLC), mobile phases composition, pH, flow rate of mobile phase, columns from different suppliers or different batches, solvents, reagents, and other material with different quality. 

Most of the above methods of column chromatography have been, or can be, automated. Devices are available for the automated application of samples to columns which are useful for analytical evaluation of samples, or for repeated analysis or separations to obtain larger amounts of material. The specific fractions of the effluent can be collected. Equipment for these purposes can be obtained from several of the supplier listed at the end of the HPLC section above with the corresponding websites. GC systems coupled with mass spectrometers (GC-MS) and HPLC systems coupled to mass spectrometers (LC-MS) are extremely important methods for the separation and identification of substances. These are invariably linked to a computer with internal libraries which can identify the peaks, and the libraries can be continually updated (see above). With more elaborate equipment LC-MS-MS where the peaks from the first spectrometer are further analysed by a second mass spectrometer provide a wealth of information. If not for the costs involved in GC-MS, GC-MS-MS, LC-MS and LC-MS-MS equipment, these systems would be more commonly found in analytical and research laboratories. [For further reading see Bibliography.]... 

Many pharmaceutical extractions do not lend themselves to simple straightforward analytical solutions. Rarely is there a case of simple extraction of a single solute from a clean feed with pure solvent. There may well be solids present which can stabilize emulsions and cause excessive entrainment. Usually, more than one solute is present, so selectivity as well as extent of extraction becomes important. Also, the solvent may contain residual solute from the solvent recovery section. Again, suppliers of extraction equipment should be contacted for their help in solving real industrial extraction problems. 

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