Keeping the spotlight on quality from a distance

 Maintaining the quality of testing in remote locations can be demanding of laboratory resources in terms of daily visits to instruments and providing support outside of normal working hours. Recently technology and software solutions have appeared to reduce this burden for laboratory scientists dramatically. The AVL Auto QC unit, in conjunction with OMNILink software, allow laboratory staff to perform many quality control and maintenance procedures on instruments in wards and medical units from a PC in the central laboratory. Assessment of this technology and software in the Special Baby Care Unit at Bradford Royal Infirmary has demonstrated many benefits including reduction in ward visits, better support out of hours, regular quality control checks, and improved analytical quality. Received: 15 April 2000 · Accepted: 15 April 2000     

An interlaboratory study to improve the quality of chemical and biological measurements in waste water

 Analyses of waste water are routinely performed to monitor the level of contamination. To verify the quality of such determinations the National Institute of Chemistry, with the support of the Ministry of Environment and Spatial Planning and the Slovenian Accreditation Agency, organizes interlaboratory comparisons. Over the last 3 years, five interlaboratory trials named "MPP-Waste Water" were organized. Each round attracted around 50 participants, mostly from Slovenia and some from abroad, which enabled the testing of SIST ISO methods or alternative methods. We prepared samples for determination of harmful substances that are important for the characterization of waste water; physico-chemical parameters (pH), global parameters – chemical oxygen demand (COD), biochemical oxygen demand (BOD₅), metals (mercury, cadmium, copper, nickel, lead and chromium (VI)), nutrients (ammonia and total phosphorus), anions (chloride, nitrite, nitrate, sulphate) and toxicity to Daphnia magna. For the analysis of each parameter we prepared two samples at two different concentration levels. The materials used in the proficiency testing were carefully prepared and their homogeneity and stability were verified. The purpose of this scheme was to enable participants to check their day-to-day analytical performance. The results should enable the participants to improve the quality of their analyses.

---

---

Received: 24 October 2002 Accepted: 2 January 2003

---

Acknowledgments We would like to thank the Ministry of Environment and Spatial Planning and the Ministry for Education, Science and Sport for providing financial support. We would like to thank members of the Technical Committee: Mrs. Marjana Kovacˇicˇ, Dr. Katja Otrin-Debevc, Prof. Dr. Marjan Veber and Mrs. Boža Gregorc for their valuable support. Special thanks are due to Dr. Adrian Van der Veen who helped us in running the first PT.

---

Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia

---

Correspondence to M. Cotman     

Proficiency test on the determination of mineral oil from polluted soils

Mineral oil products are abundant sources of environmental contamination. A Finnishproficiency test was carried out to investigate the quality of data provided in an analysis of mineral oil in polluted soils. The homogeneity and stability of the samples were tested. The calculated concentration or the median value of the results was used as the assigned value because of the unavailability of certified reference materials (CRMs). The samples were analysed using an infrared spectroscopy (IR) or gas chromatography (GC) procedure. Even if the participating laboratories had little experience with GC, the results were promising. Hence, the GC procedure will replace IR as the new ISO standard (ISO/DIS 16703) in the near future in many Finnish environmental laboratories. There is a need for CRMs for the determination of mineral oil using the GC method due to common contamination problems caused by mineral oil. Received: 9 December 2001 Accepted: 14 February 2002     

Quality management in analytical R&D in the pharmaceutical industry: Building quality from GLP

 The pharmaceutical industry is one of the most regulated activity sectors. The regulation includes specific quality systems such as good laboratory practice (GLP), good clinical practice (GCP) and good manufacture practice (GMP). The principles of GLP mainly cover the formal quality aspects of a procedure and do not evaluate the technical aspects in depth. On the other hand, EN 45001 accreditation covers technical performance and is not suitable for pharmaceutical research and development (R&D) as it is almost impossible to comply with the requirements of the European standard in the pharmaceutical environment. The challenge to the pharmaceutical industry is, therefore, to develop quality systems, compatible with GLP principles, that not only cover formal quality items but also ensure good scientific and technical performance. An implementation process focused on real quality improvement is the best way to achieve this objective, culminating in formal recognition of the quality system by third-party assessment. In the case of analytical R&D, the EURACHEM/CITAC Guide CG2 is a very good tool that can help in the definition, analysis and selection of the non GLP quality elements that will be useful. Received: 30 June 1999 / Accepted: 18 October 1999     

Reliability of food measurements: the application of proficiency testing to GMO analysis

This paper reviews the experience of the Food Analysis Performance Assessment Scheme (FAPAS^®) in operating a proficiency testing scheme for the analysis of genetically modified (GM) food. Initial rounds of proficiency testing have shown a tendency for laboratories to over-estimate GM levels, results obtained by polymerase chain reaction (PCR) and enzyme-linked immunosorbent assay (ELISA) detection methods to be significantly different and that data are skewed and not normally distributed until log-transformed. During the initial rounds, it was found that for analysis and quantification of GM material, it was not possible to assign a target value for standard deviation external to the round data, from which performance could be assessed. However, when working in a log scale, the internally derived, robust standard deviation (^σ) was found to be constant and could be used directly to predict a target value (σ) for performance assessment. Results from the first four rounds have provided valuable information and a general overview of laboratory ability. Choosing a target value for standard deviation which reflects current best practice has enabled laboratory performance to be assessed. Issues surrounding the assessment of performance are discussed which highlight some of the implications raised as a result of this initial assessment, regarding the enforcement of European labelling legislation.     

The quality of leadership (QL): the EFQM leadership criterion in relation to the 360° feedback evaluation method

The European Foundation for Quality Management (EFQM) integral quality management model covers nine issues: five so-called enabler criteria and four so-called result-oriented criteria. The first enabler criterion concerns leadership and covers all kind of strategic management aspects. However, directly or indirectly, the leadership of the board of directors or its individual members is characterized and scored. An even more explicate technique, originated in a totally different way, is the 360° feedback evaluation method. In this paper both methods are compared and practiced on various individuals. A checklist was developed to facilitate scoring in the EFQM leadership submodel. Both methods, although from a different origin, could be linked easily, covered very similar aspects and gave results that were in excellent agreement with each other. The scoring showed almost identical results, supporting in large the use of the integral EFQM model. Received: 25 May 2002 Accepted: 17 July 2002 Presented at the European Conference on Quality in the Spotlight in Medical Laboratories, 7–9 October 2001, Antwerp, Belgium Correspondence to H. M. J. Goldschmidt     

The influence of morphology on the (hydrolytic degradation of as-polymerized and hot-drawn poly(L-lactide))

 The influence of morpho-logy on the hydrolytic degradation behavior of poly(L-lactide) has been studied. High molecular weight and highly crystalline as-polymerized poly(L-lactide) was obtained in high yields through melt polymerization. Poly(L-lactide) fiber with a draw ratio of 5.6 was obtained by hot-drawing solution-spun fiber. During the bulk degradation of as-polymerized poly(L-lactide), a rapid decrease of molecular weight and tensile properties was observed. This could be explained by the morphology of the material and the presence of thermal stresses and subsequent generation of micro-cracks. The lamellar crystallites in as-polymerized poly(L-lactide) appeared to be very stable towards hydrolysis. The resorption time of high molecular weight as-polymerized poly(L-lactide) in vivo was estimated at 40–50 yr by extrapolation of molecular weight data. Hot-drawn poly(L-lactide) fiber showed exceptional hydrolytic stability under a static load and substantially retained its mechanical properties over a period of more than 5 yr. The high perfection of the crystalline fiber and the elimination of micro-voids obtained by hot-drawing prevented penetration of water and induced surface erosion of the fiber. Received: 10 February 1998 Accepted: 15 May 1998     

The performance of the rapid estimation of basis set error and correlation energy from partial charges method on new molecules of the G3/99 test set

Experimental enthalpies of formation have been approximated using single-point Hartree–Fock (HF)–self-consistent-field (SCF) total energies plus the rapid estimation of basis set error and correlation energy from partial charges (REBECEP) energy corrections. The energy corrections are calculated from the HF–SCF partial atomic charges and optimized atomic energy parameters. The performance of the method was tested on 51 closed-shell neutral molecules (50 molecules from the G3/99 thermochemistry database plus urea, composed of H, C, N, O, and F atoms). The predictive force of the method is demonstrated, because these larger molecules were not used for the optimization of the atomic parameters. We used the earlier RECEP-3 [HF/6-311+G(2d,p)] and REBECEP [HF/6-31G(d)] atomic parameter sets obtained from the G2/97 thermochemistry database (containing small molecules) together with natural population analysis and Mulliken partial charges. The best results were obtained using the natural population analysis charges, although the Mulliken charges also provide useful results. The root-mean-square deviations from the experimental enthalpies of formation for the selected 51 molecules are 1.15, 3.96, and 2.92 kcal/mol for Gaussian-3, B3LYP/6-11+G(3df,2p), and REBECEP (natural population analysis) enthalpies of formation, respectively (the corresponding average absolute deviations are 0.94, 7.09, and 2.27 kcal/mol, respectively). The REBECEP method performs considerably better for the 51 test molecules with a moderate 6-31G(d) basis set than the B3LYP method with a large 6-311+G(3df,2p) basis set. Received: 10 March 2001 / Accepted: 5 July 2001 / Published online: 11 October 2001     

The influence of shear rate, temperature and chain conformation on the critical concentration c

 When viscometry is used, a crossover phenomenon is observed separating the dilute solutions into extremely dilute solutions and dilute solutions. The critical concentration c ^**, determined from this crossover phenomenon, strongly depends on the shear rate in the solution. At very high values of shear rate the critical concentration c ^** becomes very low and depends only on the contour length of the elongated chains of different polymers. An increase of the temperature induces an increase of c ^** because the relaxation time of the chains decreases. If a polymer adopts a rodlike conformation (in a given solvent at a given temperature) the excluded volume of its chains increases and its critical concentration c ^** decreases. Received: 14 October 1996 Accepted: 3 March 1997     

A study for quality evaluation of Taxilli Herba from different hosts based on fingerprint-activity relationship modeling and multivariate statistical analysis

In this study, a fingerprint-activity relationship modeling between chemical fingerprints and antirheumatic activity was established, and multivariate statistical analysis was used to evaluate the quality of Taxilli Herba (TH) from different hosts. Characteristic fingerprints of 20 batches of TH samples were generated by high-performance liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (HPLC-Triple TOF-MS/MS), and the similarity analysis was calculated based on thirteen common characteristic peaks by hierarchical clustering analysis (HCA). Subsequently, nine efficacy markers were discovered by combining fingerprints and antirheumatic activity through grey correlation analysis (GCA) and bivariate correlation analysis (BCA). Meanwhile, the content of 5 constituents in 9 markers was determined by high-performance liquid chromatography coupled with triple quadrupole-linear ion trap tandem mass spectrometry (HPLC-QTRAP-MS/MS). The comprehensive quality of TH was assessed using multivariate statistical analysis, including principal components analysis (PCA) and technique for order preference by similarity to ideal solution (TOPSIS). The results showed that a high dose of TH extract could markedly ameliorate arthritis damage compared to other doses, with flavonoids playing an important role in the antirheumatic activity. The comprehensive quality of samples from Morus alba L. (SS) was superior to those from Liquidambar formosana Hance (FXS). The present study will demonstrate the markers associated with efficacy, and provide an applicable strategy for more comprehensive quality control and evaluation of TH.