Quality assurance systems in research and routine analytical laboratories

In our article we explain the connections between the implementation of quality assurance (QA) in research and routine analytical laboratories. J. K. Taylor claims that QA in an analytical laboratory consists of two independent but closely related terms, quality control and quality assessment. If we construct the QA system according to his ideas, problems concerning quality can be solved with only one concept regardless of the type of analytical laboratory. Therefore there is no need to introduce new QA standards for research laboratories as suggested in some papers. In the routine laboratory quality control is more important, while in the research laboratory quality assessment is dominant.     

Phoneme boundaries in normal and hearing-impaired ears

Two experiments are reported which explore variables that may complicate the interpretation of phoneme boundary data from hearing-impaired listeners. Fourteen synthetic consonant-vowel syllables comprising a/ba-da-ga/ continuum were used as stimuli. The first experiment examined the influence of presentation level and ear of presentation in normal-hearing subjects. Only small differences in the phoneme boundaries and labeling functions were observed between ears and across presentation levels. Thus monaural presentation and relatively high signal level do not appear to be complicating factors in research with hearing-impaired listeners, at least for these stimuli. The second experiment described a test procedure for obtaining phoneme boundaries in some hearing-impaired listeners that controlled for between-subject sources of variation unrelated to hearing impairment and delineated the effects of spectral shaping imposed by the hearing impairment on the labeling functions. Labeling data were obtained from unilaterally hearing-impaired listeners under three test conditions: in the normal ear without any signal distortion; in the normal ear listening through a spectrum shaper that was set to match the subject's suprathreshold audiometric configuration; and in the impaired ear. The reduction in the audibility of the distinctive acoustic/phonetic cues seemed to explain all or part of the effects of the hearing impairment on the labeling functions of some subjects. For many other subjects, however, other forms of distortion in addition to reduced audibility seemed to affect their labeling behavior.     

Analytical Uncertainty in Modern Quantitative TLC

JPC – Journal of Planar Chromatography – Modern TLC - Experiments and calculations show the importance of analytical management to reliable analytical results. A method with a...     

Separation and characterization of humic acids from Antarctica by capillary electrophoresis and matrix-assisted laser desorption ionization time-of-flight mass spectrometry. Inclusion complexes of humic acids with cyclodextrins

A new capillary electrophoresis procedure based on micellar electrokinetic capillary chromatography for the separation of humic acids (HAs) isolated from Antarctica soil was developed. The HAs were separated and characterized using a background electrolyte containing 0.09 M borate+0.09 M Tris+0.001 M EDTA (BTE) of pH 8.3, modified with alpha-, beta-, or gamma-cyclodextrins (CDs) and sodium dodecyl sulfate. It was found that from alkaline solution of HAs in the presence of CDs, the HAs are not completely precipitated with a strong acid and a certain part (some fractions) remains soluble. Mass spectrometry shows that HAs contain 15-25 simple low-Mr compounds and several families of compounds with similar structure (m/z approximately 800-1200). Comparison of HA analysis from Antarctica soil with those of soil HAs from the American continent show a high similarity between the samples and confirm several identical compounds and some with very similar structural units.     

High-performance thin-layer chromatography method for monitoring norfloxacin residues on pharmaceutical equipment surfaces

This paper presents a high-performance thin-layer chromatography (HPTLC) method with direct fluorescence measurement for the determination of norfloxacin. The method was validated for the monitoring of norfloxacin residues on stainless steel surfaces at the allowed limit of 10 mg of norfloxacin per square meter. However, it can be adapted for lower amounts of residues owing to the low detection limit of norfloxacin (about 5 ng) and can also be used for other surface materials. Test solutions were analyzed by the new HPTLC method and the known HPLC method for comparison. Accuracy and precision of the new HPTLC method, with a subsequent quantification by densitometer or video system, are comparable with those of the HPLC method.     

Determination of phenylalanine and tyrosine by liquid chromatography/mass spectrometry

Phenylketonuria is a common metabolic disorder disease. Those affected appear normal at birth, but without treatment they develop severe psychomotor retardation. Throughout life, they must control their blood levels of phenylalanine (Phe) and consume a diet containing adequate amounts of Phe and tyrosine (Tyr). We have developed a liquid chromatographic/mass spectrometric (LC/MS) method for the quantitative evaluation of Phe and Tyr in food samples. This method takes advantage of the good separation of LC and the selective and reliable quantification provided by MS in the electrospray ionization mode. The LC/MS method is very suitable for the determination of selected amino acids in various matrixes. It is sensitive to levels as low as about 0.30 ppm for Tyr and 0.70 ppm for Phe and robust. Nearly 100 nondietary food samples were analyzed by the developed method.     

The Effect of Secondary Chromatography on Quantitative TLC

Most of TLC analysis are performed in the UV and visible spectral region by measuring reflectance with a slit-scanning densitometer or a CCD camera (1-3). However, such measurements are restricted only to the surface of the TLC plate and do not take into account the vertical sub-surface concentration distribution governed by secondary chromatography (4-7) within the sorbent. It is therefore important to investigate effects connected with secondary chromatography in order to reveal their origin, and to. estimate their impact on the results of TLC measurements and their reproducibility.     

Choice of procedure conditions for radioimmunoassay of aflatoxin B1 using125I as a marker and dextrancoated charcoal as a separation matrix

Assay conditions for the radioimmunoassay for aflatoxin B₁ using¹²⁵I-radiolabel and dextran-coated charcoal for the separation of free and bound radioligand were optimized. Casein was chosen as the best protecting protein /in contrast with human serum albumin, -globulin and gelatine/. The most suitable incubation conditions are at 4°C for 18 h in darkness, radioligand sorption on the dextrancoated charcoal takes place 30 min at 4°C and the antiserum is diluted in order to reach zero specific binding in the range between 35 and 50%.     

QASKI – the quality assurance system of the National Institute of Chemistry

 The quality assurance system (QASKI) developed and implemented in the National Institute of Chemistry is presented. It tries to eliminate the incompatibilies between the present methods of quality assurance used in research and development institutes such as good laboratory practice and accreditation. Since 1991, QASKI has been used for internal accreditation of laboratories located in the institute, regardless of the fact that some of them deal with routine analyses and others with research and development. Every laboratory that wishes to ensure the credibility of its research or routine work enters QASKI and at the same time chooses an external method of approval. All interested laboratories, study directors, principal investigators, internal auditing staff, heads of documentation, quality assurance unit staff, the Director of the institute and the Quality Management Board participate in the internal system.