Matrix effects: The Achilles heel of quantitative high-performance liquid chromatography-electrospray-tandem mass spectrometry

High-performance liquid chromatography coupled by an electrospray ion source to a tandem mass spectrometer (HPLC-EST-MS/ MS) is the current analytical method of choice for quantitation of analytes in biological matrices. With HPLC-ESI-MS/MS having the characteristics of high selectivity, sensitivity, and throughput, this technology is being increasingly used in the clinical laboratory. An important issue to be addressed in method development, validation, and routine use of HPLC-ESI-MS/MS is matrix effects. Matrix effects are the alteration of ionization efficiency by the presence of coeluting substances. These effects are unseen in the chromatograrn but have deleterious impact on methods accuracy and sensitivity. The two common ways to assess matrix effects are either by the postextraction addition method or the postcolumn infusion method. To remove or minimize matrix effects, modification to the sample extraction methodology and improved chromatographic separation must be performed. These two parameters are linked together and form the basis of developing a successful and robust quantitative HPLC-EST-MS/MS method. Due to the heterogenous nature of the population being studied, the variability of a method must be assessed in samples taken from a variety of subjects. In this paper, the major aspects of matrix effects are discussed with an approach to address matrix effects during method validation proposed. (c) 2004 The Canadian Society of Clinical Chemists. All rights reserved.

Beyond winning and losing: Guidelines for evaluating high performance coaches

This paper proposes a three-step method of evaluating high performance coaches involving feedback from the athletes. First, data are collected using an instrument such as the Coaching Behavior Scale for Sport (CBS-S: Cote, Yardley, Hay, Sedgwick, & Baker, 1999). Second, a summary report is prepared with descriptive information regarding the frequency of behaviors demonstrated by the coach that can be compared to previous results or to a criterion measure. The third step involves appropriate personnel reviewing the report and subsequently providing guidance for individual coach development. This three-step appraisal method provides useful evaluative feedback to coaches and has been used in several sport programs in Canada, the United States, and Australia.

Measurement and stability of FTY720 in human whole blood by high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry

We report here a validated method for the quantification of a new immunosuppressant drug FTY720, using HPLC-tandem mass spectrometry. Whole blood samples (500 mu l) were subjected to liquid-liquid extraction, in the presence of an internal standard (Y-32919). Mass spectrometric detection was by selected reaction monitoring with an atmospheric pressure chemical ionization source in positive ionization mode (FTY720: m/z 308.3 -> 255.3). The assay was linear from 0.2 to 25 mu g/l (r(2) > 0.997, n = 5). The inter- and intra-day analytical recovery and imprecision for quality control samples (0.5, 7 and 15 mu g/l) were 95.8-103.2 and < 5.5%, respectively. At the lower limit of quantification (0.2 mu g/l) the interand intra-day analytical recovery was 99.0-102.8% with imprecision of < 7.6% (n = 5). The assay had a mean relative recovery of 100.5 +/- 5.8% (n = 15). Extracted samples were stable for 16 h. IFTY720 quality control samples were stable at room temperature for 16 h at 4 degrees C for at least 8 days and when taken through at least three freeze-thaw cycles. In conclusion, the method described displays analytical performance characteristics that are suitable for pharmacokinetic studies in humans. (c) 2006 Elsevier B.V. All rights reserved.

High performance sport coaching: Institutes of sport as sites for learning

There has been a marked increase in the number of government-funded, high performance institutes and academies of sport within Australia. Given that these organisations employ significant numbers of full-time performance sport coaches, they may be accurately characterised as workplaces. Performance sport coaches have underscored the importance of experience in developing their coaching skill. However, despite wide acceptance of the view that learning occurs everywhere but to different extents and with different efficiency, and the acknowledgement of current national coach education programs as insufficient, no sport coaching research has focused specifically on sport workplaces as sites for learning. This paper will review the current nature of coach development with a view to examining the interaction between what the workplace (institute/academy) affords the individual and the personal agency of the individual (high performance sports coaches).