Blood lead and cadmium determination: Results of the Italian external quality assessment scheme

The procedures adopted in the Italian external quality assessment scheme (EQAS) for blood Pb (B-Pb) and Cd (B-Cd) determination, including the preparation of control materials, are described. Each scheme involves the use of internal quality control materials and the participation in periodical external quality assessment trials. All control materials are prepared at the Laboratory of Clinical Biochemistry, Italian National Institute of Health (Istituto Superiore di Sanità, ISS), as the reference centre. Computerized procedures have been adopted whenever possible, i.e. sample randomization, data transfer and treatment. The analytical performance of the participating laboratories, evaluated from the results obtained in ten years of activity, is reported. A total of eight phases has been carried out between 1983 and 1993. Over the course of these ten years, a positive trend was observed for B-Pb towards a smaller bias and a lower percentage of laboratories with poor performance. In the eighth phase, taking into account the results from all participants, the mean absolute inaccuracy for B-Pb was 32 g/l (mean Pb concentration in control samples, 165 g/l). The percentage of laboratories providing results within established acceptability limits for at least 80% of the examined samples (good performers) increased with time from 28% in the first phase to 48% in the last phase. The laboratories providing less than 50% of acceptable results (poor performers) decreased from 35% in the first phase to 22% in the last phase. As regards B-Cd, mean absolute inaccuracy decreased from 0.96 g/l to 0.55 g/l between the first phase and the sixth phase. The percentage of good performers increased from 45% to 62% and that of poor performers decreased from 31% to 5%. From the seventh phase a large group of new laboratories agreed to participate in the EQAS for B-Cd and the inaccuracy rose to 0.75 g/l (mean concentration: 2.7 g/l) and the percentage of poor performers rose to 24%, whereas the percentage of good performers remained almost unchanged.     

Reference materials and analytical standards to stimulate improved laboratory performance: Experience from the external quality assessment scheme for trace elements in biological samples

The performance of a large number of laboratories measuring trace elements in biological fluids has been monitored over many years by examination of their results in the Guildford external quality assessment scheme. Specific experiences of the UK trace elements reference laboratories have been used to stimulate improvements in performance of other participants in the scheme. The key features of these initiatives were: specially prepared reference materials, used as internal quality control specimens within a common procedure, contributed to accuracy control; proposed standards of satisfactory and unacceptable analytical performance associated with a new system for scoring; regular non-threatening open discussion of performance with interested colleagues. The impact of these features is illustrated with reference to measurements of Al and Zn in serum and Pb in whole blood.     

Quality specifications for evaluation and comparison of performance among external quality assessment schemes in occupational and environmental laboratory medicine

Quality specifications (QS) are proposed for lead in blood and for aluminium, copper, selenium and zinc in serum as part of the aim to set standards of performance for laboratories so that results can be demonstrated to be fit for the purpose to which they are applied. The QS were established taking account of the analytical state-of-the-art, physiological variations in the concentrations of the analyte and the clinical purpose for which the assay is to be used. A procedure was devised that uses these QS to give equivalence of assessment among external quality assessment schemes (EQAS), thus avoiding conflicting information which has been demonstrated in the past. Advantages of this procedure are: to provide direct comparison of performance of laboratories taking part in different schemes, to provide equivalence of assessment of laboratory performance necessary to establish mutual recognition agreements, and to demonstrate the fitness for purpose of results from participants.Presented at the Eurachem PT Workshop September 2005, Portorož, Slovenia     

External quality assessment in microbiology: comparison of results from Belgian and Canadian laboratories with regard to their ability to identify <Emphasis Type="Italic">Streptococcus pyogenes</Emphasis>

Clinical Microbiology Proficiency Testing (CMPT; Canada) and the Institute of Public Health (IPH; Belgium) set up a joint external quality assessment (EQA) project in which they sent identical simulated clinical samples to their respective participants. Samples were sent out as throat swabs containing Streptococcus pyogenes (as pathogen) and viridans streptococci (as commensal). Results from identification by the Belgian laboratories were excellent: 99.5% detected the group A streptococci. About 10% of the Canadian laboratories reported the absence of reportable β-haemolytic streptococci, although for most of them the issue was one of non-examination of small or pin-point streptococci. Overall, Canadian and Belgian laboratories performed well in this EQA; the joint project clearly showed that although many similarities exist, there are differences between laboratories in treating EQA samples and reporting results.     

Geospatial and statistical approaches to nitrate health risk and groundwater quality assessment of an alluvial aquifer in SE Nigeria for drinking and irrigation purposes

In agricultural districts, like Ogbaru in southeastern Nigeria, water supplies are under obvious threats from human activities. Therefore, continuous monitoring and assessment of water quality suitability for drinking, domestic, and irrigation purposes are encouraged to keep check of the effects of water contaminants. In this paper, several quality water assessment tools were integrated to determine the suitability of the groundwater in Ogbaru for drinking and irrigation uses and to assess the ingestion and dermal health risks of nitrate occurrence. The majority of the physicochemical parameters analyzed in this study were within their respective standard limits. However, groundwater quality index classified 52.63% of the groundwaters as excellent water and 47.37% as good water. Overall index of pollution, on the other hand, classified 84.21% as excellent water and 15.79% as acceptable water. The pH ranged from 5.4 to 6.8, indicating that the groundwater is acidic. Most irrigation water quality assessment indices (SAR, Na%, PS, KR, RCO, CAI-1 and 2) revealed that the groundwater samples are suitable for irrigation. However, magnesium hazard and permeability index grouped the majority of the water samples as unsuitable resources for irrigation uses. The nitrate health risk assessment (mean score = 1.371) indicated that children are exposed to higher non-carcinogenic health risk due to ingestion of contaminated groundwater than the other populations. It was observed that 21.05% of the groundwater samples had the highest concentrations of the analyzed chemical species. Multivariate statistical methods (hierarchical cluster analysis and factor analysis) efficiently aided the contaminant source apportionment. Based on the findings of this paper, it is advised that adequate regulatory strategies and water treatment techniques be adopted in the area to protect and sustain the groundwater quality and public health.     

Standardization and validation of phytometabolites by UHPLC and high-performance thin layer chromatography for rapid quality assessment of ancient ayurvedic medicine,Mahayograj Guggul

Mahayograj Guggul is an ancient ayurvedic medicine, prescribed for various joint disorders like arthritis, gout, and rheumatism. The present research was envisaged to develop a simple, sensitive, and comprehensive analytical method for standardization of Mahayograj Guggul. The analysis was conducted for gallic acid, protocatechuic acid, vanillic acid, cinnamic acid, piperine, guggulsterone-E, and guggulsterone-Z by high-performance thin-layer chromatography, and additionally ferulic acid, ellagic acid, and picroside I by ultra high-performance liquid chromatography. These developed methods were validated as per international guidelines, and were found linear (r² > 0.99), sensitive, precise (relative standard deviation < 5%), and accurate with recovery values (85–105%). The limit of detection and quantification were in the range of 0.11–23.6 and 0.33–71.51 μg/g. Gas chromatography tandem mass spectrometry was used to develop Mahayograj Guggul fingerprinting profile and to identify mid-polar or nonpolar compounds. Proximate analysis was used to ascertain the functional groups present in Mahayograj Guggul. Ultra high-performance liquid chromatography and gas chromatography tandem mass spectrometry were further employed to authenticate quality reproducibility in the active ingredients of Mahayograj Guggul in six commercial batches. Taken together, these analytical methods provide a scientific basis and reference for quality control evaluation of Mahayograj Guggul and similar traditional broad-spectrum formulations.     

Fingerprint and multicomponent quantitative analysis for the quality evaluation of Sibiraea angustata leaves by HPLC-DAD and HPLC-ESI-MS/MS combined with chemometrics

Sibiraea angustata leaves, known as a traditional Tibetan medicine, have been specially used in the treatment of indigestion and obesity. In the study, a simple and sensitive high-performance liquid chromatography (HPLC) method with a diode array detector (DAD) was established to solve the problem of lacking quality standard of S. angustata leaves, including the fingerprint analysis and quantification of six characteristic components. The analytical method was validated for linearity, repeatability, stability, recovery, and specificity. Seventeen raw samples and 1 processed sample of S. angustata leaves were collected from different locations of China to establish the fingerprint. The chemometric methods, including similarity analysis (SA), principal component analysis (PCA), and hierarchical clustering analysis (HCA), were applied to distinguish the 18 batches of S. angustata samples. The results successfully sorted these samples into five clusters and kept in line with each other. According to the result of the fingerprint analysis, 21 peaks were extracted to be the common peaks and most of them were identified by mass spectrometry (MS) with electron-spray ionization (ESI) in the negative mode. Meanwhile, the loading plot of PCA further indicated that the peaks of neochlorogenic acid, chlorogenic acid, ferulic acid, rutin, hyperin, and isoquercitrin played a greater role in the discrimination among the 21 peaks. So the six components mentioned above were investigated as index constituents to evaluate the quality of S. angustata leaves from different locations. The study demonstrated that the developed new method was a beneficial approach for authentication and quality evaluation of S. angustata leaves.     

Chemical profiling by LC–MS/MS and HPLC fingerprint combined with chemometrics and simultaneous determination of 16 characteristic ingredients for the quality consistency evaluation of Shaoyao‐Gancao Decoction

In this paper, to evaluate the effect of the region of origin on the quality consistency of Shaoyao‐Gancao Decoction (SGD), the SGD fingerprint was developed for the first time. Chemometric methods including similarity analysis, hierarchical clustering analysis and principal component analysis were employed to study the quality consistency of SGD. Meanwhile, high‐performance liquid chromatography coupled with electrospray ionization quadrupole time‐of‐flight mass spectrometry was applied for comprehensive analysis of SGD and 93 compounds were tentatively characterized. Furthermore, a high‐performance liquid chromatography method with multi‐wavelength switching for simultaneous determination of 16 characteristic ingredients comprising gallic acid, oxypaeniflorin, albiflorin, paeoniflorin, liquiritin apioside, liquiritin, isoliquiritin apioside, galloylpaeoniflorin, 1,2,3,4,6‐penta‐O‐galloyl‐d ‐galactopyranose (PGG), ononin, isoliquiritin, liquiritigenin, benzoylpaeoniflorin, glycyrrhizic acid, isoliquiritigenin and formononetin, was established. All 16 analytes show excellent linearity (R² ≥ 0.9990) with recoveries ranging from 96.58 to 104.61% and limits of detection and quantification of 0.022–0.291 and 0.037–0.635 μg/mL, respectively. Finally, it was successfully applied to determine 15 batches of SGD. The results of our research indicate that different regions of origin have a significant effect on the quality consistency of SGD, and its fingerprint combined with chemometrics and multi‐ingredient determination comprise an efficient and reliable approach for quality consistency evaluation.