Essential steps to providing reliable results using the Analytical Quality Assurance Cycle

Considering how demand for quality assurance (QA) has grown in analytical laboratories, we show the trends in analytical science, illustrated through international standard ISO/IEC 17025, validation, measurements of uncertainty, and quality-control (QC) measures. A detailed review of the history of analytical chemistry indicates that these concepts are consistently used in laboratories to demonstrate their traceabilities and competences to provide reliable results. We propose a new approach for laboratory QA, which also develops a diagram to support routine laboratories (which generally apply a quality system, such as ISO/IEC 17025) or research laboratories (that have some difficult applying this international standard). This approach, called the Analytical Quality Assurance Cycle (AQAC), presents the major QA concepts and the relationships between these concepts in order to provide traceability and reliable results. The AQAC is a practical tool to support the trend towards QA in analytical laboratories. (C) 2012 Elsevier Ltd. All rights reserved.

Validação de métodos analíticos - estudos de casos relevantes de atividades dos laboratórios de controle de qualidade de vacinas

A validação dos métodos de análises em situações fora da rotina, em P&D pesquisa e desenvolvimento, pode tornar-se um processo de difícil solução, em oposição àquelas de rotina, onde as concentrações são conhecidas. Nesta última situação, o método analítico é validado e aprovado com simplicidade. Apesar dos elementos de qualidade básicos para análises em P&D serem os mesmos adotados nas análises de rotina, fatores como o comportamento imprevisível da amostra, a composição desconhecida da matriz e interdependência com o analito, mesmo a incerteza a respeito da escolha do método instrumental, requer uma atenção renovada nos elementos de qualidade existentes. A razão pode ser atribuída à imprevisibilidade do procedimento analítico e a extensão do esforço adicional dos elementos de qualidade. As incertezas das análises em P&D requerem uma cuidadosa consideração do problema, assim como a disponibilidade de técnicas analíticas. Ao mesmo tempo, devem-se observar o planejamento e organização do trabalho, a supervisão do desenvolvimento analítico e a adequação dos aspectos técnico e organizacional - no trabalho de P&D, a definição de responsabilidades e a competência do corpo técnico. A garantia da qualidade nas indústrias farmacêuticas é estabelecida pelo desenvolvimento de especificações apropriadas para matérias-primas, produtos intermediários e produtos finais. A importância de especificações adequadas foi estabelecida e exemplos foram dados no desenvolvimento de especificação típica para produtos farmacêuticos, tais como a vacina e matéria prima. Isto incluiu uma discussão dos tipos de parâmetros que precisam ser controlados e uma indicação dos valores numéricos ou faixas esperadas para muitos materiais utilizados. A metrologia analítica que necessita ser aplicada para demonstrar a observância com as especificações foi discutida, com as implicações de desempenho do método para diferenciar variações na qualidade do produto e a simples variabilidade analítica. Esse trabalho foi escrito para laboratórios, com a finalidade de dar um suporte na implementação da validação de métodos analíticos e introduzir o conceito de incerteza da medida nas análises de rotina. O objetivo foi fornecer de uma maneira compreensível e prática a metodologia dos cálculos das medidas de incerteza baseados principalmente em dados de controle de qualidade e de validação já existentes. Exemplos práticos retirados diretamente do Laboratório de Metrologia e Validação, FIOCRUZ / Bio-Manguinhos, foram apresentados. Entretanto, o tratamento usado neste trabalho é genérico e pode ser aplicável a outros laboratórios químicos

Palmyra Atoll coral reef habitat mapping completion report

The United States Coral Reef Task Force (USCRTF) was established in 1998 by Presidential Executive Order 13089 to lead U.S. efforts to preserve and protect coral reef ecosystems. Current, accurate, and consistent maps greatly enhance efforts to preserve and manage coral reef ecosystems. With comprehensive maps and habitat assessments, coral reef managers can be more effective in designing and implementing a variety of conservation measures, including: • Long-term monitoring programs with accurate baselines from which to track changes; • Place-based conservation measures such as marine protected areas (MPAs); and • Targeted research to better understand the oceanographic and ecological processes affecting coral reef ecosystem health. The National Oceanic and Atmospheric Administration’s (NOAA) National Ocean Service (NOS) is tasked with leading the coral ecosystem mapping element of the U.S. Coral Reef Task Force (CRTF) under the authority of the Presidential Executive Order 13089 to map and manage the coral reefs of the United States.

Implementation of a quality system in joint master programmes

Joint master programmes are systems which by default demand a proper quality system in order to sustain and improve. Objective of this thesis is analysing and proposing solutions to difficulties associated with the implementation of a quality management system to joint master programmes, with the focus on international joint master programmes. The application of the analysis to the Erasmus Mundus joint master programme European Master in Quality in Analytical Laboratories (EMQAL) is discussed. QA systems implementation in HEIs in Europe is an ongoing process, and implementation of such systems in JPs is one step further to enhancing quality in higher education in Europe. The issue closely discussed in this thesis is: should QMS be developed independently from the institutions, or should the institutions, when developing their quality management systems, take into account the (future) development of joint courses and prepare their quality procedures accordingly? A quality management system is normally developed for one organization, and different aspects of cooperation are considered within. A joint master programme is a result of successful cooperation of two or more organizations; therefore a development of its quality management system must be approached in a different manner. This thesis proposes a QMS with emphasis both on the HEI and the consortium. Different processes in the QMS can be managed independently at the level of the HEI or at the level of the consortium. Most processes in joint master programmes should be designed in programmes’ and institutions’ QMSs. Quality of a joint master programme cannot be analyzed separately from the higher education institutions which are organizing it. Comparative analysis of organization of one Erasmus Mundus Master programme to the solutions proposed in discussion showed that from all of the aspects considered, processes in EMQAL are organized in harmony with the proposed delegation of processes of the QMS for a joint master programme. The solutions proposed in the discussion are based on theoretical application of the quality principles and concepts. Comparison to the quality processes and procedures in an existing EM programme showed that analysis is applicable in practice.

Head Space-Trap GC-MS method development and validation for the analysis of volatile organic compounds in water samples

Dissertação de Mestrado, Qualidade em Análises, Faculdade de Ciências e Tecnologia, Universidade do Algarve, 2015

Evaluation of NRC, UC Davis and ADAS approaches to estimate the metabolizable energy values of feeds at maintenance energy intake from equations utilizing chemical assays and in vitro determinations

Feed samples received by commercial analytical laboratories are often undefined or mixed varieties of forages, originate from various agronomic or geographical areas of the world, are mixtures (e.g., total mixed rations) and are often described incompletely or not at all. Six unified single equation approaches to predict the metabolizable energy (ME) value of feeds determined in sheep fed at maintenance ME intake were evaluated utilizing 78 individual feeds representing 17 different forages, grains, protein meals and by-product feedstuffs. The predictive approaches evaluated were two each from National Research Council [National Research Council (NRC), Nutrient Requirements of Dairy Cattle, seventh revised ed. National Academy Press, Washington, DC, USA, 2001], University of California at Davis (UC Davis) and ADAS (Stratford, UK). Slopes and intercepts for the two ADAS approaches that utilized in vitro digestibility of organic matter and either measured gross energy (GE), or a prediction of GE from component assays, and one UC Davis approach, based upon in vitro gas production and some component assays, differed from both unity and zero, respectively, while this was not the case for the two NRC and one UC Davis approach. However, within these latter three approaches, the goodness of fit (r(2)) increased from the NRC approach utilizing lignin (0.61) to the NRC approach utilizing 48 h in vitro digestion of neutral detergent fibre (NDF:0.72) and to the UC Davis approach utilizing a 30 h in vitro digestion of NDF (0.84). The reason for the difference between the precision of the NRC procedures was the failure of assayed lignin values to accurately predict 48 h in vitro digestion of NDF. However, differences among the six predictive approaches in the number of supporting assays, and their costs, as well as that the NRC approach is actually three related equations requiring categorical description of feeds (making them unsuitable for mixed feeds) while the ADAS and UC Davis approaches are single equations, suggests that the procedure of choice will vary dependent Upon local conditions, specific objectives and the feedstuffs to be evaluated. In contrast to the evaluation of the procedures among feedstuffs, no procedure was able to consistently discriminate the ME values of individual feeds within feedstuffs determined in vivo, suggesting that the quest for an accurate and precise ME predictive approach among and within feeds, may remain to be identified. (C) 2004 Elsevier B.V. All rights reserved.

The epidemiology of ecstasy use and harms in New South Wales, Australia

Aims:This paper examines the epidemiology of ecstasy use and harm in Australia using multiple data sources.

Design: The data included (1) Australian Customs Service 3,4-methylenedioxymethamphetamine (MDMA) detections; (2) the National Drug Strategy Household and Australian Secondary Student Alcohol and Drug Surveys; (3) data from Australia's ecstasy and Related Drugs Reporting System; (4) the number of recorded police incidents for ecstasy possession and distribution collated by the N.S.W. Bureau of Crime Statistics and Research; (5) the number of calls to the Alcohol and Drug Information Service and Family Drug Support relating to ecstasy; (6) the Alcohol and Other Drug Treatment Services National Minimum Dataset on number of treatment episodes for ecstasy, and (7) N.S.W. Division of Analytical Laboratories toxicology data on number of deaths where MDMA was detected.

Findings: Recent ecstasy use among adults in the general population has increased, whereas among secondary students it has remained low and stable. The patterns of ecstasy consumption among regular ecstasy users have changed over time. Polydrug use and use for extended periods of time (>48 h) remain common among this group. Frequent ecstasy use is associated with a range of risk behaviours and other problems, which tend to be attributed to a number of drugs along with ecstasy. Few ecstasy users present for treatment for problems related to their ecstasy consumption.

Conclusions: Messages and interventions to reduce the risks associated with polydrug use and patterns of extended periods of use are clearly warranted. These messages should be delivered outside of traditional health care settings, as few of these users are engaged with such services.

Treatment of 1,10-phenanthroline laboratory wastewater using the solar photo-Fenton process

The red Fe2+-phenanthroline complex is the basis of a classical spectrophotometric method for determination of iron. Due to the toxicity of this complexing agent, direct disposal of the wastewaters generated in analytical laboratories is not environmentally safe. This work evaluates the use of the solar photo-Fenton process for the treatment of laboratory wastewaters containing phenanthroline. Firstly, the degradation of phenanthroline in water was evaluated at two concentration levels (0.1 and 0.01%, w/v) and the efficiencies of degradation using ferrioxalate (FeOx) and ferric nitrate were compared. The 0.01% w/v solution presented much higher mineralization, achieving 82% after 30 min of solar irradiation with both iron sources. The solar photo-Fenton treatment of laboratory wastewater containing, in addition to phenanthroline, other organic compounds such as herbicides and 4-chlorophenol, equivalent to 4500 mg L-1 total organic carbon (TOC) resulted in total degradation of phenanthroline and 25% TOC removal after 150 min, in the presence of either FeOx or ferric nitrate. A ratio of 1: 10 dilution of the residue increased mineralization in the presence of ferrioxalate, achieving 38% TOC removal after 120 min, while use of ferric nitrate resulted in only 6% mineralization over the same period. (c) 2007 Elsevier B.V. All rights reserved.

Analytical strategies to solve problems in industrial and official laboratories

210 p.

Organic Contaminant Analytical Methods of the National Status and Trends Program: 2000-2006

This document describes the analytical methods used to quantify core organic chemicals in tissue and sediment collected as part of NOAA’s National Status and Trends Program (NS&T) for the years 2000-2006. Organic contaminat analytical methods used during the early years of the program are described in NOAA Technical Memoranda NOS ORCA 71 and 130 (Lauenstein and Cantillo, 1993; Lauenstein and Cantillo, 1998) for the years 1984-1992 and 1993-1996, respectively. These reports are available from our website (http://www.ccma.nos.gov) The methods detailed in this document were utilized by the Mussel Watch Project and Bioeffects Project, which are both part of the NS&T program. The Mussel Watch Project has been monitoring contaminants in bivalves and sediments since 1986 and is the longest active national contaminant monitoring program operating in U.S. costal waters. Approximately 280 Mussel Watch sites are sampled on a biennial and decadal timescale for bivalve tissue and sediment respectively. Similarly, the Bioeffects Assessment Project began in 1986 to characterize estuaries and near coastal environs. Using the sediment quality triad approach that measures; (1) levels of contaminants in sediments, (2) incidence and severity of toxicity, and (3) benthic macrofaunal conmmunities, the Bioeffects Project describes the spatial extent of sediment toxicity. Contaminant assessment is a core function of both projects. These methods, while discussed here in the context of sediment and bivalve tissue, were also used with other matricies including: fish fillet, fish liver, nepheloid layer, and suspended particulate matter. The methods described herein are for the core organic contaminants monitored in the NS&T Program and include polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), butyltins, and organochlorines that have been analyzed consistently over the past 15-20 years. Organic contaminants such as dioxins, perfluoro compounds and polybrominated biphenyl ethers (PBDEs) were analyzed periodically in special studies of the NS&T Program and will be described in another document. All of the analytical techniques described in this document were used by B&B Laboratories, Inc, an affiliate of TDI-Brook International, Inc. in College Station, Texas under contract to NOAA. The NS&T Program uses a performance-based system approach to obtain the best possible data quality and comparability, and requires laboratories to demonstrate precision, accuracy, and sensitivity to ensure results-based performance goals and measures. (PDF contains 75 pages)

Sampling and analytical methods of the National Status and Trends Program Mussel Watch Project: 1993-1996 Update

Polycyclic aromatic hydrocarbons, butyltins, polychlorinated biphenyls, DDT and metabolites, other chlorinated pesticides, trace and major elements, and a number of measures of contaminant effects are quantified in bivalves and sediments collected as part of the NOAA National Status and Trends (NS&T) Program. This document contains descriptions of some of the sampling and analytical protocols used by NS&T contract laboratories from 1993 through 1996. (PDF contains 257 pages)

20th annual meeting of the WEFTA Working Group on Analytical Methods in Fish and Fishery Products and 3rd annual meeting of the WEFTA Working Group on Microbiology. A retrospect on 20 years

After 20 annual meetings it is worth to have a look back and to see how it has started. There has been very little collaboration on research projects between member institutes under the auspices of WEFTA, co-operation in more neutral areas of common interest was developed at an early stage. The area which has proved very fruitful is methodology. It was agreed that probably the best way to make progress was to arrange meetings at each laboratory in turn where experienced, practising scientists could describe in detail how they carried out analyses. In this way, difficulties could be demonstrated or uncovered, and the accuracy, precision, efficiency and cost of the methods used in different laboratories could be compared.