System suitability samples

Go back to a documented reference point by performing a system check with a test mix or system suitability sample that can lead to a quick diagnosis. 

The following notes should be given due consideration when evaluating a system suitability sample. 

Limited sample clean-up could overload the analytical column, and residual matrix components can accumulate on the column after multiple injections. The residual matrix components can also solidify and deposit over a period of time in the LC-MS ionization source or vacuum interface, resulting in a decrease in ion transfer efficiency. The decrease in instrumentation performance (i. e., signal intensity) can be monitored by the signals of system-suitability samples dispersed within an analytical batch. The practice of replacing the pre-column in every run and scrubbing the analytical column periodically with a cleaning mobile phase will help to maintain instrument performance. 

System Suitability Sample o CS and QC a Coded Incurred Sample Normal Incurred Sample... 

Another example in regard to in situ degradation for generation of a system suitability sample is given in the literature [24],... 

Detailed method. The method procedure should be unambiguous with example chromatograms of the standard, a typical sample, and a system suitability sample with example calculations. 

When using this technique, the most appropriate wavelength is selected from the UV spectrum of the pure compound and that of the system suitability sample. Usually, the A ax is chosen however, in order to remove unwanted interference, it may be necessary to move away from this value. Where possible, the use of wavelength <250 nm should be avoided because of the high level of background interference and solvent adsorption. In practical terms, this requires the use of far-UV grade solvents and the avoidance of organic buffers. 

In this work there is proposed approach which allows using broad standar ds for calibration and system suitability test. The approach is based on main principle of using of standards i.e. maximal closeness of tested sample and standar d. It has been shoved that the approach allows achieving essential improvement of robustness of method for determination of MWD of dextrans. 

For construction of suitable samples molecular beam epitaxy was selected, the method of choice for the production of complicated epitaxial layer systems with different materials. As substrates Si wafer material (about 20x20 mm-, thickness 1 mm) and SiO, discs (diameter 30 mm, thickness 3 mm) were used. Eight layered structures (one, two and three layers) were built up with Al, Co, and Ni, with an indicated thickness of 70 nm, each. 

Of all the requirements that have to be fulfilled by a manufacturer, starting with responsibilities and reporting relationships, warehousing practices, service contract policies, airhandUng equipment, etc., only a few of those will be touched upon here that directly relate to the analytical laboratory. Key phrases are underlined or are in italics Acceptance Criteria, Accuracy, Baseline, Calibration, Concentration range. Control samples. Data Clean-Up, Deviation, Error propagation. Error recovery. Interference, Linearity, Noise, Numerical artifact. Precision, Recovery, Reliability, Repeatability, Reproducibility, Ruggedness, Selectivity, Specifications, System Suitability, Validation. 

In case of reduced availability of an impurity a possible approach is to prepare a spiked sample , i.e. a known amount of impurity is added to the CRS and may serve in a system suitability test as well as for the control of the level of this impurity. An example is given in the monograph for chlorprothixene hydrochloride (Monograph 0815 1999) where the content of the E-isomer is controlled to a level of not more than 2 per cent, Figure 5.5. 

Sample preparation techniques vary depending on the analyte and the matrix. An advantage of immunoassays is that less sample preparation is often needed prior to analysis. Because the ELISA is conducted in an aqueous system, aqueous samples such as groundwater may be analyzed directly in the immunoassay or following dilution in a buffer solution. For soil, plant material or complex water samples (e.g., sewage effluent), the analyte must be extracted from the matrix. The extraction method must meet performance criteria such as recovery, reproducibility and ruggedness, and ultimately the analyte must be in a solution that is aqueous or in a water-miscible solvent. For chemical analytes such as pesticides, a simple extraction with methanol may be suitable. At the other extreme, multiple extractions, column cleanup and finally solvent exchange may be necessary to extract the analyte into a solution that is free of matrix interference. 

There are two uses of chemical standards in chemical analysis. In the first place, they may be used to verify that an instrument works correctly on a day-to-day basis - this is sometimes called System Suitability checking. This type of test does not usually relate to specific samples and is therefore strictly quality assurance rather than quality control. Secondly, the chemical standards are used to calibrate the response of an instrument. The standard may be measured separately from the samples (external standardization) or as part of the samples (internal standardization). This was dealt with in Section 5.3.2. 

Regular calibration and verification ensures that the parameters measured by a particular instrument can be related to a recognized standard. The frequency of instrument calibration may be quite varied, depending largely on the application. If, during the verification of instrument performance, it has been shown that the instrument stays in calibration for about three months, the calibration would be repeated at approximately two-monthly intervals. However, verification (system suitability) will be carried out each time samples are analysed. For some critical analyses, calibration may be performed for each batch of samples or, in an extreme case, for each separate sample. 

System Suitability is another aspect of the LOD testing. With any quantitative TLC experiment, the LOD sample is typically applied in addition to any standards or samples to ensure it can be seen under the conditions of the lab on that given day, and that system suitability has been established. 

In the new Stratus CS system results are available in less than 15 min after sample draw and the system has the capability to analyze four samples in less than 30 min. Ease of use, analytical sensitivity, accuracy, precision, and reproducibility makes this system suitable for use in chest pain centers, emergency departments, critical care units, observation wards and clinical laboratories. 

System suitability tests serve to define the level of electrophoretic performance necessary to ensure valid CE assay results. System suitability of the method was evaluated by analyzing the symmetry of the IB-367 peak, theoretical plates of the capillary, and resolution between IB-367 and IB-300, the closest peak to IB-367. The sample concentration of the method was selected at approximately 0.5 mg/ml to assure symmetry below 3.5 and to assume sufficient sensitivity for detecting low... 

For the purpose of sample introduction, any sample introduction system (also sample inlet system or inlet) suitable for the respective compound can be employed. Hence, direct probes, reservoir inlets, gas chromatographs and even liquid chromatographs can be attached to an El ion source. Which of these inlet systems is to be preferred depends on the type of sample going to be analyzed. Whatever type the inlet system may be, it has to manage the same basic task, i.e., the transfer of the analyte from atmospheric conditions into the high vacuum of the El ion source Table 5.1 provides an overview. 

---