<p>The purpose of our study has been to examine the methods of validation and reminiscences from an employee point of view. To answer our aim a qualitative disquisition with four assistant nurses and one pedagogue in craft was conducted. The result was divided into three different themes: the view on people with dementia, merits and demerits with the methods and to work with people with dementia. The analysis of the result was made from selected parts of the system theory and symbolic interaction theory.</p><p>The result of our disquisition can be summarized in that all our interviewed persons above all only can see advantages with the methods and several express that they are good tools to use in their work with people with dementia. The majority of our interviewed persons make use of the methods in everyday, spontaneous, meetings with the elderly. Everyone mentions the workgroup as an important factor in the work with the validation and reminiscence methods. Some experience a support in their work from their colleagues while others feel themselves being impeded.</p>

The purpose of our study has been to examine the methods of validation and reminiscences from an employee point of view. To answer our aim a qualitative disquisition with four assistant nurses and one pedagogue in craft was conducted. The result was divided into three different themes: the view on people with dementia, merits and demerits with the methods and to work with people with dementia. The analysis of the result was made from selected parts of the system theory and symbolic interaction theory. The result of our disquisition can be summarized in that all our interviewed persons above all only can see advantages with the methods and several express that they are good tools to use in their work with people with dementia. The majority of our interviewed persons make use of the methods in everyday, spontaneous, meetings with the elderly. Everyone mentions the workgroup as an important factor in the work with the validation and reminiscence methods. Some experience a support in their work from their colleagues while others feel themselves being impeded.

Polycyclic Aromatic Hydrocarbons (PAHs) are one of the pollutants in the environment. They are organic compounds that consist of more than one aromatic ring (Kanchanamayoon & Tatrahun 2008). Due to less information forthcoming regarding the levels of PAHs in Vaal area, this study is to evaluate the levels of PAHs in the rivers around Vaal Triangle. Three river sites such as Vaal, Barrage and Klip Rivers were selected to investigate the concentration of polycyclic aromatic hydrocarbons in water. Validation of an analytical method is the process by which it is established by laboratory studies, that the performance characteristics of the method meet the requirements for the intended analytical application. (Stockl et al 2009). The validation parameters tested were, linearity detection limit of quantitation, sensitivity, accuracy, specificity, selectivity, robustness and ruggedness. PAHs can be determined using High Performance Liquid Chromatography (HPLC) which is a technique for separation, identification and quantification of components in a mixture. The following ten compounds were identified and quantified with a HPLC: naphthalene, acenaphthylene, phenanthrene, anthracene, fluoranthene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h) anthracene and indeno(1,2,3-cd)pyrene. The linear calibration ranges from 0.1-5ppm.The linearity ranges between 0.9993-0.9999.Three reversed sorbent phases (Strata-X, MFC18 and C18) were tested for PAH retention efficiency. An optimised reverse solid phase extraction (SPE) method was used after conditioning the sorbent to extract and collect compounds of polycyclic aromatic hydrocarbons (PAHs) in river water samples. LC18 sorbent showed good recoveries after extracting PAHs standard mixture of 1 mg/l. The best performing eluting solvent was acetonitrile and very good percentage recoveries that ranged from 70% to over 100 % were obtained for eight compounds. Poor recoveries were also obtained for phenanthrene (61%) and benzo(b)fluoranthene (48%). The standard deviation ranged from 0.01 to 0.05 and the detection limits ranging from 0.01 – 0.17 mg/l were obtained. Average concentration ranges of PAHs identified within the study area were: phenanthrene (0.02 – 0.42 mg/l); anthracene (0.37 – 0.39 mg/l), fluoranthene (0.11 – 0.15 mg/l); benzo(b)fluoranthene (0.09 mg/l) and indeno(1,2,3-cd)pyrene (0.26 mg/l). However, naphthalene, acenaphthylene, benzo(k)fluoranthene, benzo(a)pyrene and dibenzo(a,h)anthracene were not detected.

The quality of food is an increasingly important matter of concern in Europe. The feeding stuffs poisoning episode that occurred in Belgium in May 1999 pointed out the vulnerability of the food chain and the lack of appropriate monitoring. Polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and polychlorobiphenyls (PCBs) were the key contaminants involved. This has triggered new EU legislation, including maximum and action limits for relevant food and feed products as well as requirements for analytical method used to verify compliance. Large monitoring programs to test food and feed have been launched and, in many countries, efforts to monitor dioxins and related compounds strongly increased. To cope with the large number of samples statistically required for monitoring, the recommanded strategy involves the use of screening methods based on low resolution mass spectrometry (LRMS) and/or bio-assays, and high resolution mass spectrometry (HRMS) method, used to bear out their presence. Major analytical challenges had to be met to face with the large number of samples including the authoritys requests on developing screening and alternative methods for monitoring programs of PCDD/Fs and PCBs in food and feed. The first part of this document is devoted to the development of an alternative LRMS-based method for PCDD/Fs and PCBs measurement in food and feed. The second part of this thesis is an answer to the basic questions commonly addressed to all analytical chemists developing method but here in a particular context due to very specific family of compounds involved: How to make sure that my method is able to achieve sufficient accuracy on results? Are there any analytical benchmarks available for validation purposes? How to evaluate measurement uncertainty expressed in toxic equivalent (TEQ) units? How to report results right? How can the proficiency of my laboratory be measured? To ensure the quality of data obtained, laboratories in charge of the food control on PCDD/Fs and dioxin-like PCBs encounter a number of severe problems. One has to mention the lack of sufficient and reliable certified reference materials that are necessary to validate methods, too scarce data available on current analytical method performances, and the absence of quality criteria approach for analytical method. During the course of this work, I contributed to answer these questions to the general analytical effort by providing useful tools and methodologies. At that time, straightforward answers could not be found in the scientific literature. One of the reasons was the scarce data of dioxins in food and feed available. One can also mention the unusual part the dioxins play in chemical analysis. Indeed, the main features that characterize a dioxin measurement are the low levels at which these compounds occur in biological samples (sub parts-per-trillion), levels that are currently not explored by any other applications in chemical analysis in the food sector and therefore the difficulty to cope with precision models available; the reporting of results expressed in total tetrachloro dibenzo-p-dioxin (TCDD) toxic equivalent concentration for compliance assessment with statutory limits; and, what necessarily follows from the decision-making: the statement of the uncertainty interval also expressed in toxic units. To answer the foregoing questions in an international frame, notions such as validation of analytical procedures, fitness for purpose, internal quality control, interlaboratory studies, proficiency testing, measurement uncertainty, traceability had to be introduced. They are all encompassed in the analytical quality assurance management a laboratory should implement. These concepts are strongly connected to statistical techniques. This branch of analytical chemistry that consists in extracting relevant information from data using statistical and mathematical methods adapted to the specific needs for the chemists is called chemometrics. Quality is an essential preoccupation of chemometrics but it cannot be only limited to these aspects. Chemometrics relates also to other topics such as experiments and experimental design methodologies, (new) knowledge about chemical systems. Chemometrics and quality This thesis treats several aspects and new approaches of quality assurance for an ultra-trace contaminant laboratory: external method validation through interlaboratory studies and estimation of repeatability, reproducibility and trueness using simple statistics based on normal distributions (ISO 5725) but also more complex statistical tests for heavily tailed, skewed or even bimodal distributions; the production and the use of a reference material for internal validation and internal quality control (QC) purposes; advanced statistics in quality control chart and multi-level control charts for sensitive detection of bias; proposal of quality criteria for assessment of proficiency of dioxin laboratories; proposal of benchmark precision for internal validation purposes; estimation of measurement uncertainty. The thesis is divided in the following chapters: Chapter 1 is a general introduction for dioxins and related compounds. It consists of a brief introduction to general characterization, mechanism of toxicity, human exposure and European legislation in food and feed. Chapter 2 provides an overview of the analytical procedures for mass spectrometry based methods. It gives a brief summary of the most frequently used techniques to extract and purify PCDDs, PCDFs and dioxin-like PCBs (DL-PCBs) from food and feed matrices. Regarding detection, special attention of the principles of detection and quantification by HRMS in selected ion monitoring mode (SIM) and the quadrupole ion storage low resolution mass spectrometer in MS/MS mode is addressed. Chapter 3 discusses the development and optimization of a large volume injection (LVI)-gas chromatography (GC)-ion trap MS/MS method as an alternative to GC-HRMS for the measurement of PCDD/Fs in food and feed. Instrumental detection limits were lowered by a factor 2 to 3 with the development, in collaboration with the manufacturer, of a system of damping gas pressure inside the trap that improves precursor ions trapping efficiency. We achieved 5:1 signal to noise with the injection of 200 fg of 2,3,7,8 TCDD. With slight adjustments to sample size and final extract volume, we demonstrated on QC samples the good agreement between this method and the reference GC/HRMS method for PCDD/Fs and DL-PCBs in food and feed. In chapter 4, the first European inter-laboratory study on dioxins, furans and dioxin-like PCBs using the HRGC/HRMS method in animal feed samples is described with two main objectives. The first objective was to produce a reference material for internal validation and QC purposes. The second objective was to assess the analytical performances of the GC-HRMS method close to maximum levels as no data were available at that time and to check whether EU directives requirements were met. Chapter 5 is a general discussion on the capability of the state-of-the-art HRGC/HRMS method to provide reliable results at decreasing maximum levels. Levels have to decrease according to EU policy regarding human exposure to those contaminants. In this case, we present the issue from a different angle, i.e. the analytical point of view for the future establishment of target levels. Based on the results of PCDD/Fs and DL-PCBs interlaboratory study in animal feedingstuffs described in chapter 4, we demonstrated for the sum of the 17 PCCD/Fs toxic congeners that reliable results can be easily provided up to a value of 0.17 ng WHO-TEQ/kg. The ability to reliably quantify a minute trace of these contaminants has been pointed out with the aim of providing an analytical benchmark for the future establishment of target dioxin levels in animal feedingstuffs. Hence, both analytical and toxicological aspects should be examined together to set realistic target levels achievable for most dioxin laboratories involved in monitoring programs. One of the central themes of this thesis is the establishment of an empirical relationship between reproducibility standard deviation and the dioxin congeners level in food and feed. Chapter 6 deals with raw data from numerous performances interlaboratory studies of PCDD/Fs and DL-PCBs in food and feed. Striking linear functions in log scale between reproducibility standard deviation and congeners level over a concentration range of 10-8 to 10-14 g per g fresh weight were observed. The data fit very well to a Horwitz-type function of the form sR = 0.153c0.904, where sR and c are dimensionless mass ratios expressed in pg/g on fresh weight, regardless of the nature of the toxic congeners, food and feed matrices, or sample preparation methods. I called this relationship the dioxin function. One of the main features of the dioxin function could be its use as a suitable fitness-for-purpose criterion for dioxins and related compounds in proficiency testing (PT) exercises. We illustrated its use with practical example with data from the largest international PT in this field. Another application is its use as benchmark precision criteria for internal validation. Chapter 7 discusses the role of internal quality control (IQC) to monitor analytical processes. Introducing new QC methods derived from the industrial practice to analytical chemistry, improving data evaluation and allowing to detect shifts or trends, are elements that are difficult to point out with classical approach (Shewhart chart). The importance of ARL (average run length) as a key-criteria of the efficiency of a quality control procedure will be emphasized. The introduction of the multivariate approach of multilevel control with the Hotelling's T2-test will lead to a better detection of random errors than the independently managed conventional Shewhart charts. Moreover, the Exponentially Weighted Moving Average (EWMA) will offer a flexible tool for detecting the inacurracy of a method, especially where small shifts or bias are of interest. All these concepts, recently introduced in clinical chemistry, were applied here for the monitoring of PCDD/Fs and DL-PCBs in food and feed. Chapter 8 introduces the concept of measurement uncertainty (MU). Three top-down approaches for uncertainty estimation are proposed on the example of the GC-HRMS method for PCDD/Fs and DL-PCBs in various food and feed matrices: the approach which combines long-term precision and trueness data to obtain an estimate of MU (Barwick and Ellision method); the approach which uses the reproducibility estimate from interlaboratory-studies as uncertainty estimate; the concept of accuracy profile used in the context of validation and internal quality control to assess MU. Chapter 9 presents a general conclusion

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / Este trabalho teve como objetivo o desenvolvimento e metodologia cromatogrÃfica para a determinaÃÃo de bisfenol A em quatro diferentes simulantes de alimentos utilizando cromatografia lÃquida de alta eficiÃncia e detector de arranjo de diodo (PDA) para suporte em enasios de migraÃÃo. Os simulantes utilizados foram A (Ãgua purificada), B (soluÃÃo aquosade Ãcido acÃtico a 3%), C (soluÃÃo aquosa de etanol a 10%) e D (soluÃÃo aquosa de etanol a 95%). A avaliaÃÃo preliminar das condiÃÃes de anÃlise foi conduzida com a finalidade de estabelecer aquelas que conferem os melhores resultados, os quais foram o sistema de fase mÃvel acetonitrila-Ãgua na proporÃÃo volumÃtrica 70:30, temperatura de 40ÂC do forno da coluna e comprimento de onda em 201 nm. O tempo de retenÃÃo do bisfenol A encontrado foi de 3,25 minutos. Para os simulantes, o mÃtodo de tratamento consistiu da evaporaÃÃo de 1 ml de amostra amostra a 60ÂC com duraÃÃo de 1 hora e 45 minutos (A e C), 2 horas (B) e 1 hora (D). Em sequÃncia, o mÃtodo foi avaliado com relaÃÃo aos parÃmetros de validaÃÃo analÃtica, incluindo linearidade, limite de detecÃÃo e de quantificaÃÃo, repetibilidade, precisÃo intermediÃria entre analistas diferentes e entre dias diferentes, recuperaÃÃo,seletividade e robustez. O mÃtodo desenvolvido para o simulante A apresentou coeficiente de determinaÃÃo (rÂ) 0,9988 ou superior no intervalo testado (50 a 2000 ppb); limite de detecÃÃo e de quantificaÃÃo , respectivamente, 14,7 ppb e 48,9 ppb; coeficiente de variaÃÃo para repetibilidade de 2,07%, para a precisÃo inter-dias de 1,05% e para a precisÃo inter-analistas de 1,76%; recuperaÃÃo de 97,9% (CV= 1,3%) (50 ppb), 99,2% (CV= 0,7%) (1000 ppb) e 103,6% (CV= 0,4%). Os resultados obtidos para o simulante B incluem coeficiente de determinaÃÃo (rÂ) 0,9972 ou superior; limite de detecÃÃo e de quantificaÃÃo, respectivamente, 7,8 ppb e 26,0 ppb; coeficientes de variaÃÃo para repetibilidade de 3,74%, precisÃo inter-dias de 0,14% e precisÃo inter-analistas de 0,2%; recuperaÃÃo de 94,8% (CV= 4,8%) (50 ppb), 99,8% (CV= 0,2%) (1000 ppb) e 92,3% (CV= 1,2%) (2000 ppb). Para o simulante C os resultados incluem coeficiente de determinaÃÃo (rÂ) 0,9988 ou superior; limite de detecÃÃo e de quantificaÃÃo, respectivamente, 4,8 ppb e 16,1 ppb; coeficiente de variaÃÃo para repetibilidade de 2,84%, precisÃo inter-dias de 1,37%e precisÃo inter-analistas de 0,14%; recuperaÃÃo de104,6% (CV= 2,5%) (50 ppb), 99,8% (CV= 1,3%) (1000 ppb) e 102,5% (CV= 2,9%) (2000 ppb). Os resultados para o simulante D foram r 0,9984 ou superior; limite de detecÃÃo e de quantificaÃÃo,respectivamente, 13,7 ppb e 45,6 ppb; coeficiente de variaÃÃo para repetibilidade de 2,0%, precisÃo inter-dias de 1,9% e precisÃo inter-analistas de1,2%; recuperÃÃo de 92,6% (CV= 1,76%) (50 ppb), 99,9% (CV= 0,9%) (1000 ppb) e 104,8% (CV= 2,7%) (2000 ppb). NÃo foram observados interferentes importantes para o mÃtodo testado, mostrando-se robusto. / This study aimed to develop and chromatographic method for the determination of bisphenol A in four different food simulants using high performance liquid chromatography and diode array detector (PDA) to support in enasios migration. The simulating used were A (purified water), B (solution aquosade 3% acetic acid), C (aqueous 10% ethanol) and D (aqueous 95% ethanol). Preliminary assessment of the analytical conditions was conducted in order to establish those that confer the best results, which were the system of mobile phase acetonitrile-water in the ratio 70:30 by volume, 40  C oven and length of the column wavelength of 201 nm. The retention time of the bisphenol A was found to be 3.25 minutes. For simulating the method of treatment consists of evaporation of sample 1 ml of sample at 60  C with duration of 1 hour and 45 minutes (A and C), 2 hours (B) and 1 hour (D). In sequence, the method was evaluated with respect to the parameters of analytical validation, including linearity, limit of detection and quantification, repeatability, intermediate precision between different analysts and between different days, recovery, selectivity and robustness. The method for simulating the coefficient for determining (r Â) or greater than 0.9988 in the range tested (50 to 2000 ppb); detection limit and quantitation, respectively, 14.7 ppb and 48.9 ppb; coefficient variation in repeatability of 2.07% for the inter-day precision of 1.05% and the accuracy of inter-Analyst 1.76%, recovery of 97.9% (CV = 1.3%) (50 ppb ), 99.2% (CV = 0.7%) (1000 ppb) and 103.6% (CV = 0.4%). The results for the simulant B includes coefficient of determination (r Â) 0.9972 or higher; limit of detection and quantification, respectively, 7.8 ppb and 26.0 ppb; coefficients of variation for repeatability of 3.74%, inter day precision, accuracy and 0.14% cross-Analyst 0.2%, 94.8% recovery (CV = 4.8%) (50 ppb) and 99.8% (CV = 0.2% ) (1000 ppb) and 92.3% (CV = 1.2%) (2000 ppb). For the simulant C results include a coefficient of determination (r Â) 0.9988 or higher; limit of detection and quantification, respectively, 4.8 ppb and 16.1 ppb, coefficient of variation for repeatability of 2.84%, accuracy inter-day precision of 1.37% and inter-analysts of 0.14%; de104 recovery, 6% (CV = 2.5%) (50 ppb), 99.8% (CV = 1.3%) ( 1000 ppb) to 102.5% (CV = 2.9%) (2000 ppb). The results for simulating D was 0.9984 r  or more, detection limit and quantitation, respectively, 13.7 ppb and 45.6 ppb; coefficient of variation of 2.0% to repeatability, accuracy of an inter-day 9% and accurate inter-de1 analysts, 2%; recuperÃÃo 92.6% (CV = 1.76%) (50 ppb) and 99.9% (CV = 0.9%) (1000 ppb) and 104 8% (CV = 2.7%) (2000 ppb). There were no significant interferences to the method tested and proved to be robust.

LINHARES JUNIOR, Gilberto Ferreira. Desenvolvimento e validação de metodologia cromatográfica para determinação de bisfenol A em simulantes de alimentos de ensaios de migração. 2012. 101 f. : Dissertação (mestrado) - Universidade Federal do Ceará, Centro de Ciências Agrárias, Departamento de Tecnologia de Alimentos, Fortaleza-CE, 2012 / Submitted by Nádja Goes (nmoraissoares@gmail.com) on 2016-06-08T15:09:14Z No. of bitstreams: 1 2012_dis_gflinharesjunior.pdf: 1691103 bytes, checksum: 0abb8d914beb4b36dee06bc962679c7b (MD5) / Approved for entry into archive by Nádja Goes (nmoraissoares@gmail.com) on 2016-06-08T15:09:30Z (GMT) No. of bitstreams: 1 2012_dis_gflinharesjunior.pdf: 1691103 bytes, checksum: 0abb8d914beb4b36dee06bc962679c7b (MD5) / Made available in DSpace on 2016-06-08T15:09:30Z (GMT). No. of bitstreams: 1 2012_dis_gflinharesjunior.pdf: 1691103 bytes, checksum: 0abb8d914beb4b36dee06bc962679c7b (MD5) Previous issue date: 2012 / This study aimed to develop and chromatographic method for the determination of bisphenol A in four different food simulants using high performance liquid chromatography and diode array detector (PDA) to support in enasios migration. The simulating used were A (purified water), B (solution aquosade 3% acetic acid), C (aqueous 10% ethanol) and D (aqueous 95% ethanol). Preliminary assessment of the analytical conditions was conducted in order to establish those that confer the best results, which were the system of mobile phase acetonitrile-water in the ratio 70:30 by volume, 40 ° C oven and length of the column wavelength of 201 nm. The retention time of the bisphenol A was found to be 3.25 minutes. For simulating the method of treatment consists of evaporation of sample 1 ml of sample at 60 ° C with duration of 1 hour and 45 minutes (A and C), 2 hours (B) and 1 hour (D). In sequence, the method was evaluated with respect to the parameters of analytical validation, including linearity, limit of detection and quantification, repeatability, intermediate precision between different analysts and between different days, recovery, selectivity and robustness. The method for simulating the coefficient for determining (r ²) or greater than 0.9988 in the range tested (50 to 2000 ppb); detection limit and quantitation, respectively, 14.7 ppb and 48.9 ppb; coefficient variation in repeatability of 2.07% for the inter-day precision of 1.05% and the accuracy of inter-Analyst 1.76%, recovery of 97.9% (CV = 1.3%) (50 ppb ), 99.2% (CV = 0.7%) (1000 ppb) and 103.6% (CV = 0.4%). The results for the simulant B includes coefficient of determination (r ²) 0.9972 or higher; limit of detection and quantification, respectively, 7.8 ppb and 26.0 ppb; coefficients of variation for repeatability of 3.74%, inter day precision, accuracy and 0.14% cross-Analyst 0.2%, 94.8% recovery (CV = 4.8%) (50 ppb) and 99.8% (CV = 0.2% ) (1000 ppb) and 92.3% (CV = 1.2%) (2000 ppb). For the simulant C results include a coefficient of determination (r ²) 0.9988 or higher; limit of detection and quantification, respectively, 4.8 ppb and 16.1 ppb, coefficient of variation for repeatability of 2.84%, accuracy inter-day precision of 1.37% and inter-analysts of 0.14%; de104 recovery, 6% (CV = 2.5%) (50 ppb), 99.8% (CV = 1.3%) ( 1000 ppb) to 102.5% (CV = 2.9%) (2000 ppb). The results for simulating D was 0.9984 r ² or more, detection limit and quantitation, respectively, 13.7 ppb and 45.6 ppb; coefficient of variation of 2.0% to repeatability, accuracy of an inter-day 9% and accurate inter-de1 analysts, 2%; recuperção 92.6% (CV = 1.76%) (50 ppb) and 99.9% (CV = 0.9%) (1000 ppb) and 104 8% (CV = 2.7%) (2000 ppb). There were no significant interferences to the method tested and proved to be robust. / Este trabalho teve como objetivo o desenvolvimento e metodologia cromatográfica para a determinação de bisfenol A em quatro diferentes simulantes de alimentos utilizando cromatografia líquida de alta eficiência e detector de arranjo de diodo (PDA) para suporte em enasios de migração. Os simulantes utilizados foram A (água purificada), B (solução aquosade ácido acético a 3%), C (solução aquosa de etanol a 10%) e D (solução aquosa de etanol a 95%). A avaliação preliminar das condições de análise foi conduzida com a finalidade de estabelecer aquelas que conferem os melhores resultados, os quais foram o sistema de fase móvel acetonitrila-água na proporção volumétrica 70:30, temperatura de 40°C do forno da coluna e comprimento de onda em 201 nm. O tempo de retenção do bisfenol A encontrado foi de 3,25 minutos. Para os simulantes, o método de tratamento consistiu da evaporação de 1 ml de amostra amostra a 60°C com duração de 1 hora e 45 minutos (A e C), 2 horas (B) e 1 hora (D). Em sequência, o método foi avaliado com relação aos parâmetros de validação analítica, incluindo linearidade, limite de detecção e de quantificação, repetibilidade, precisão intermediária entre analistas diferentes e entre dias diferentes, recuperação,seletividade e robustez. O método desenvolvido para o simulante A apresentou coeficiente de determinação (r²) 0,9988 ou superior no intervalo testado (50 a 2000 ppb); limite de detecção e de quantificação , respectivamente, 14,7 ppb e 48,9 ppb; coeficiente de variação para repetibilidade de 2,07%, para a precisão inter-dias de 1,05% e para a precisão inter-analistas de 1,76%; recuperação de 97,9% (CV= 1,3%) (50 ppb), 99,2% (CV= 0,7%) (1000 ppb) e 103,6% (CV= 0,4%). Os resultados obtidos para o simulante B incluem coeficiente de determinação (r²) 0,9972 ou superior; limite de detecção e de quantificação, respectivamente, 7,8 ppb e 26,0 ppb; coeficientes de variação para repetibilidade de 3,74%, precisão inter-dias de 0,14% e precisão inter-analistas de 0,2%; recuperação de 94,8% (CV= 4,8%) (50 ppb), 99,8% (CV= 0,2%) (1000 ppb) e 92,3% (CV= 1,2%) (2000 ppb). Para o simulante C os resultados incluem coeficiente de determinação (r²) 0,9988 ou superior; limite de detecção e de quantificação, respectivamente, 4,8 ppb e 16,1 ppb; coeficiente de variação para repetibilidade de 2,84%, precisão inter-dias de 1,37%e precisão inter-analistas de 0,14%; recuperação de104,6% (CV= 2,5%) (50 ppb), 99,8% (CV= 1,3%) (1000 ppb) e 102,5% (CV= 2,9%) (2000 ppb). Os resultados para o simulante D foram r² 0,9984 ou superior; limite de detecção e de quantificação,respectivamente, 13,7 ppb e 45,6 ppb; coeficiente de variação para repetibilidade de 2,0%, precisão inter-dias de 1,9% e precisão inter-analistas de1,2%; recuperção de 92,6% (CV= 1,76%) (50 ppb), 99,9% (CV= 0,9%) (1000 ppb) e 104,8% (CV= 2,7%) (2000 ppb). Não foram observados interferentes importantes para o método testado, mostrando-se robusto.