9 resultados para Internal standard

em Deakin Research Online - Australia


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A simple and rapid method for the analysis of carbohydrates in heroin samples by capillary electrophoresis utilizing a borate complexation method is described. Separations were performed using an uncoated fused silica capillary, 50 cm × 50 mm I.D. × 360 mm O.D. with an effective separation length of 9 cm. The system was run at 60°C with an applied voltage of -8 kilovolts. Injection of each sample was for 1 sec at -50 mbar. UV detection was employed with the wavelength set at 195 nm. The background electrolyte consisted of 65 mM borate, pH 12.0. Samples and standards were prepared in the run buffer containing 2 mg/mL of mannose as an internal standard. Under these conditions a test mixture containing glucose, sucrose, lactose, mannitol and mannose as an internal standard was resolved within 5 min. The method was used to determine the concentration of carbohydrates in heroin seizure samples and synthetic heroin samples. The results were in good agreement with the reported values.

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A simple and rapid method for the analysis of heroin seizures by micellar electrokinetic chromatography with short-end injection is described. Separations were performed using an uncoated fused silica capillary, 50 cm×50 mm I.D.×360 mm O.D. with an effective separation length of 8 cm. The system was run at 25°C with an applied negative voltage of –25 kilovolts. Injection of each sample was for 2 s at –50 mbar. UV detection was employed with the wavelength set at 210 nm. The background electrolyte consisted of 85:15 (water:acetonitrile, v/v) containing final concentrations of 25 mM SDS and 15 mM sodium borate, pH 9.5. Samples and standards were prepared in 0.1% v/v acetic acid and diluted in the run buffer containing 1 mg/ml of N,N-dimethyl-5-methoxytryptamine as an internal standard. Under these conditions a text mixture containing caffeine, paracetamol, morphine, codeine, heroin, and acetylcodeine was resolved within 1.5 min. The method was used to determine the concentration of heroin in heroin seizure samples, and the results were in good agreement with those obtained by a validated gas chromatographic method.

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A simple and sensitive HPLC method was developed to simultaneously determine CPT-11 and its major metabolite SN-38 in culture media and cell lysates. Camptothecin (CPT) was used as internal standard (I.S.). Compounds were eluted with acetonitrile–50 mM disodium hydrogen phosphate buffer containing 10 mM sodium 1-heptane-sulfonate, with the pH adjusted to 3.0 using 85% (w/v) orthophosphoric acid (27/73, v/v) by a Hyperclon ODS (C18) column (200 mm × 4.6 mm i.d.), with detection at excitation and emission wavelengths of 380 and 540 nm, respectively. The average extraction efficiencies were 96.9–108.3% for CPT-11 in culture media and 94.3–107.2% for CPT-11 in cell lysates; and 87.7–106.8% for SN-38 in culture media and 90.1–105.6% for SN-38 in cell lysates. Within- and between-day precision and accuracy varied from 0.1 to 10.3%. The limit of quantitation (precision and accuracy <20%) was 5.0 and 2.0 ng/ml for CPT-11 and 1.0 and 0.5 ng/ml for SN-38 in culture media and cell lysates, respectively. This method was successfully applied to quantitate the cellular accumulation and metabolism of CPT-11 and SN-38 in H4-II-E, a rat hepatoma cell line.

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Irinotecan (CPT-11) and its main metabolite SN-38 are potent anticancer derivatives of camptothecin (CPT), with active lactone and inactive carboxylate forms coexisting. A simple and sensitive HPLC method using the ion-pairing reagent tetrabutylammonium hydrogen sulfate (TBAHS) was developed to simultaneously determine all four analytes in rat plasma samples. Camptothecin (CPT) was used as internal standard. The mobile phase was 0.1 M potassium dihydrogen phosphate containing 0.01 M TBAHS (pH 6.4)–acetonitrile (75:25, v/v). Separation of the compounds was carried out on a Hypersil C18 column, monitored at 540 nm (excitation wavelength at 380 nm). All four compounds gave linear response as a function of concentration over 0.01–10 μM. The limit of quantitation in rat plasma was 0.01, 0.008, 0.005 and 0.005 μM for CPT-11 lactone, CPT-11 carboxylate, SN-38 lactone and SN-38 carboxylate, respectively. The method was successfully used in the study on the effect of coadministered thalidomide on the plasma pharmacokinetics of CPT-11 and SN-38 in rats. Coadministered thalidomide (100 mg/kg body weight by intraperitoneal injection) significantly increased the AUC0–10h values of CPT-11 lactone and CPT-11 carboxylate by 32.6% and 30.3 %, respectively, (P < 0.01), but decreased the values by 19.2% and 32.4% for SN-38 lactone and carboxylate, respectively, (P < 0.05). Accordingly, the value of total body clearance (CL) of CPT-11 lactone was significantly lower in combination group compared to the control (1.329 versus 1.837 L/h/kg, P = 0.0002). Plasma t1/2β values for SN-38 lactone and carboxylate were significantly (P < 0.01) smaller in rats with coadministered thalidomide, as compared to rats receiving CPT-11 alone. Further studies are needed to explore the underlying mechanisms for the observed kinetic interaction between CPT-11 and thalidomide.

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Optimal plant growth is the result of the interaction of a complex network of plant hormones and environmental signals. Ascorbic acid (AsA) is a crucial antioxidant in plants and is involved in the regulation of cell division, cell expansion, photosynthesis and hormone biosynthesis. Quantitative analysis of AsA in Arabidopsis thaliana organs was conducted using HPLC with d -isoascorbic acid (Iso-AsA) as an internal standard. Analysis revealed Àuctuations in the levels of AsA in different organs and growth phases when plants were grown under standard conditions. AsA concentrations increased in leaves in direct proportion to leaf size and age. Young siliques (seed set stage) and Àowering buds (open and unopened) showed the highest levels of AsA. A relationship was found between the level of AsA and indole acetic acid (IAA) in leaves, stems, Àowers, and siliques and the highest level of IAA and AsAwere found in the Àowers. In contrast, the lowest level of the plant hormone, salicylic acid, was found in the Àowers and the highest quantity measured in the leaves. Consequently, AsA has been found to be a multifunctional molecule that is involved as a key regulator of plant growth and development.

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Background and Purpose: The impact of stroke is multidimensional however standard stroke measures do not discriminate well when stroke patients are less physically impaired. The Stroke Impact Scale 2.0 (SIS 2.0) is a multidimensional measure of the impact of stroke but its'' psychometric properties require further testing. The SIS-16 is a measure of physical functioning designed to be more sensitive to differences in physical functioning than current stroke outcome measures but there is only preliminary information detailing its'' reliability and validity. The current study examined the internal consistency and validity of the SIS 2.0 and SIS-16 in an Australian sample of stroke patients. Methods: The SIS 2.0, SIS-16, World Health Organization Bref-Scale (WHOQOL-BREF) and Zung''s Self-Rating Depression Scale (SDS) were completed by 74 stroke patients in rural Victoria, Australia.
Results: The item convergent validity index indicated good item convergence of the SIS-16 and SIS 2.0 domains. The item discriminant validity index had only adequate divergence for most SIS 2.0 domains. Internal consistencies of the SIS-16 and SIS 2.0 domains were acceptable (agr = 0.87–0.95). Correlations between the SIS-16 and SIS 2.0 and the WHOQOL-BREF and SDS supported the convergent and discriminant validity of the SIS-16 and all the dimensions of the SIS 2.0 except lsquoParticipationrsquo which lacked discriminant validity. Conclusions: The SIS 2.0 and SIS-16 had good psychometric properties with support for the internal consistency and validity of both measures.

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This thesis describes research that was conducted into the potential of modeling the activities of the Data Processing Department as an aid to the computer auditor. A methodology is composed to aid in the evaluation of the Internal Controls, particularly the General Controls relative to computer processing. Consisting of three major components, the methodology enables the auditor to model the presumed activities of the Data Processing Department against the actual activities, as recorded on the Operating System Log. The first component of the methodology is the construction and loading of a model of the presumed activities of the Data Processing Department from its verbal, scheduled, and reported activities. The second component is the generation of a description of the actual activities of the Data Processing Department from the information recorded on the Operating System Log. This is effected by reducing the Operating System Log to the format described by the Standard Audit File concept. Finally, the third component in the methodology is the modeling process itself. This is in fact a new analysis technique proposed for use by the EDP auditor. The modeling process is composed of software that compares the model developed and loaded in the first component, with the description of actual activity as collated by the second component. Results from this comparison are then reviewed by the auditor, who determines if they adequately depict the situation, or whether the models description as specified in the first component requires to be altered, and the modeling process re-initiated. In conducting the research, information and data from a production installation was used. Use of the ‘real-world’ input proved both the feasibility of developing a model of the reported activities of the Data Processing Department, and the adequacy of the operating system log as a source of information to report the departments actual activities. Additionally, it enabled the involvement and comment of practicing auditors. The research involved analysis of the effect of EDP on the audit process, structure of the EDP audit process, data reduction, data structures, model formalization, and model processing software. Additionally, the Standard Audit File concept was verified through its use by practising auditors, and expanded by the development of an indexed data structure, which enabled its analysis to be conducted interactively. Results from the trial implementation of the research software and methodology at a production installation confirmed the research hypothesis that the activities of the Data Processing Department could be modelled, and that there are substantial benefits from the EDP auditor in analysing this process. The research in fact provides a new source of information, and develops a new analysis technique for the EDP auditor. It demonstrates the utilization of computer technology to monitor itself for the audit function, and reasserts auditor independence by providing access to technical detail describing the processing activities of the computer.

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Purpose – Accounting and water industry experts are developing general-purpose water accounting (GPWA) to report information about water and rights to water. The system has the potential to affect water policies, pricing and management, and investment and other decisions that are affected by GPWA report users' understanding of water risks faced by an entity. It may also affect financial returns to accounting and auditing firms and firms in water industries. In this paper the authors aim to examine the roles of the accounting profession, water industries and other stakeholders in governing GPWA. Recognising that the fate of GPWA depends partly upon regulatory power and economics, they seek to apply regulatory theories that explain financial accounting standards development to speculate about the national and international future of GPWA.

Design/methodology/approach – Official documents, internal Water Accounting Standards Board documents and unstructured interviews underpin the authors' analysis.

Findings – The authors speculate about the benefits that might accrue to various stakeholder groups from capturing the GPWA standard-setting process. They also suggest that internationally, water industries may dominate early GPWA standards development in the public interest and that regulatory capture by accounting or water industry professionals will not necessarily conflict with public interest benefits.

Practical implications – Accounting for water can affect allocations of environmental, economic, social and other resources; also, accounting and water industry professional standing and revenues. In this paper the authors identify factors influencing GPWA standards and standard-setting institutional arrangements, and thereby these resource allocations. The paper generates an awareness of GPWA's emergence and practical implications.

Originality/value –
This is an early study to investigate water accounting standard-setting regulatory influences and their impact.

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Purpose: The purpose of this study is to investigate the impact of internal control weaknesses on accounting conservatism in Chinese listed firms. It also investigates the relationship between the demand for external audit and accounting conservatism, and whether additional assurance of internal control reports (ICRs) can mitigate the negative impact of ICWs on accounting conservatism.

Design/methodology/approach:
An empirical research approach is taken through the use of ordinary least squares (OLS) models and hand-collected internal control weakness data from ICRs released by Chinese listed firms.

Findings: The results of this paper show that the existence of ICWs has a negative effect on accounting conservatism in China. Further, the results demonstrate that both accounting-related and non-accounting-related ICWs affect accounting conservatism. The authors also find that there is a complementary relationship between accounting conservatism and the demand for additional assurance of ICRs, and additional assurance of ICRs can mitigate the negative impact of ICWs on accounting conservatism.

Practical Implications: This study provides timely evidence to Chinese regulators of the possible economic consequences of the official implementation of internal control standard in China from 2012. The findings of this paper can also benefit regulators around the world and, in particular, the regulators in emerging markets that are considering implement regulations similar to the US SOX.

Originality/value:
The paper demonstrates that a wider scope of ICWs, including non-accounting-related ICWs, also has a significant impact on accounting conservatism. Therefore, this research provides a more general evidence on the relationship between internal control quality and accounting conservatism.