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Validation Parameters (validation + parameter)
Selected AbstractsCapillary high performance liquid chromatography coupled with electrospray ionization mass spectrometry for rapid analysis of pinane monoterpene glycosides in Cortex MoutanJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1 2008Yue Song Abstract In this study, a rapid and reliable assay has been developed for quantification of pinane monoterpene glycosides in Cortex Moutan; it is based on capillary high performance liquid chromatography coupled with electrospray ionization mass spectrometry (capillary HPLC,ESI MS). This method utilizes capillary HPLC for the separation of seven pinane monoterpene glycosides in a methanol extract of the botanical sample followed by negative ion electrospray ionization and single ion monitoring (SIM). The compounds of interest in the sample were unambiguously identified on the basis of information about retention time and quasi-molecular ions ([M,H],) or adduct ions ([M+HCOO],). Validation parameters of the method were established. The linearity range was 1.01,105.5 ,g/mL with the square of correlation coefficients lying in the range of 0.9965,0.9997, limits of detection were on the fmol level, the average recoveries varied between 91.8 and 101.0%, and good precision values (RSD, 1.2,4.91%) for peak area were obtained. After validation, the applicability of the method for determination of these pinane monoterpene glycosides in Cortex Moutan has been demonstrated. [source] Validation of a real-time PCR for the quantitative estimation of a G143A mutation in the cytochrome bc1 gene of Pyrenophora teresPEST MANAGEMENT SCIENCE (FORMERLY: PESTICIDE SCIENCE), Issue 3 2007Arash Kianianmomeni Abstract A single nucleotide polymorphism (SNP) in the cytochrome b gene confers resistance to strobilurin fungicides for several fungal pathogens. Therefore, on the basis of a change at amino acid position 143 from glycine to alanine, a real-time PCR assay was established for the quantitative detection of the analogous SNP in the cytochrome b sequence of Pyrenophora teres Drechsler, which causes barley net blotch. Allelic discrimination was achieved by using allele specific primers with artificially mismatched nucleic acid bases and minor groove binding probes. Validation parameters for the lower limits of the working range, namely limits of detection (LOD) and limits of quantification (LOQ), were statistically determined by the variance of calibration data, as well as by the variance of the 100% non-strobilurin-resistant allele DNA sample (blank values). It was found that the detection was limited by the variance of blank values (five in 801 458 copies; 0.0006%), whereas the quantification was limited by the variance of calibration data (37 in 801 458 copies; 0.0046%). The real-time PCR assay was finally used to monitor strobilurin-resistant cytochrome b alleles in barley net blotch field samples, which were already classified in in vivo biotests to be fully sensitive to strobilurins. All signals for strobilurin-resistant cytochrome b alleles were below the LOD, and therefore the results are in total agreement with the phenotypes revealed by biotests. Copyright © 2006 Society of Chemical Industry [source] Tocopherols and tocotrienols in grape seeds from 14,cultivars grown in KoreaEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 12 2009Minjung Wie Abstract In this study, the tocopherol (T) and tocotrienol (T3) contents of grape seeds from 14 different varieties grown in Korea were analyzed using saponification extraction followed by normal-phase liquid chromatography. ,-T, ,-T, ,-T3, and ,-T3 were detected in all samples. The total concentration of tocopherol and tocotrienol was in the range of 4.8,9.9,mg/100,g seed (35.3,68.8,mg/100,g oil basis). The Muscat Bailey,A cultivar had the highest total tocopherol and tocotrienol contents, followed by Canner and Naples. ,-T3 ranged from 1.6 to 4.9,mg/100,g seed (11.2 to 53.81,mg/100,g oil basis) and was the main isomer, followed by ,-T3 in most of the samples. Analytical method validation parameters including accuracy and precision were determined. Overall recovery from grape seeds was close to 100%. [source] Comparison of immunoradiometric assays for determination of thyroglobulin: a validation studyJOURNAL OF CLINICAL LABORATORY ANALYSIS, Issue 3 2007L.A. Tortajada-Genaro Abstract In this study we compared and validated commercial immunoradiometric assays (IRMA) to determine thyroglobulin (Tg) levels in serum. From a set of 440 samples, 68 were selected to calculate the validation parameters and the clinical performance of the assays. The commercial kits evaluated were the Tg-CTK (DiaSorin), IRMAZenco Tg (ZenTech), and SELco-Tg (Medipan). We found that 21% of the collected samples were in the critical range of concentration. Detection limits were calculated as being below 3,µg/L. Intra- and inter-reproducibility were lower than 3.1% and 9.2%, respectively. Dilution and recovery studies provided quantitative determinations. Correlation regression coefficients from the results of the methods were obtained. The determined concentrations were compared with the clinical evidence of disease. Variation in the 125-iodine-labeled antibody concentration and control charts showed the robustness of the methods. Analysis time and the simplicity of the methods were also evaluated. Reliable Tg determination is important for monitoring patients with differentiated thyroid cancer (DTC), controlling other thyroid diseases, and assessing the quality of imaging techniques. A strategy for verification and comparison based on analytical parameters and clinical performance is proposed. J. Clin. Lab. Anal. 21:147,153, 2007. © 2007 Wiley-Liss, Inc. [source] Irinotecan and its active metabolite, SN-38: review of bioanalytical methods and recent update from clinical pharmacology perspectivesBIOMEDICAL CHROMATOGRAPHY, Issue 1 2010Mullangi Ramesh Abstract The introduction of irinotecan has revolutionized the applicability of camptothecins as predominant topoisomerase I inhibitor for anti-cancer therapy. The potent anti-tumor activity of irinotecan is due to rapid formation of an in vivo active metabolite, SN-38. Therefore, irinotecan is considered as a pro-drug to generate SN-38. Over the past decade, side-by-side with the clinical advancement of the use of irinotecan in the oncology field, a plethora of bioanalytical methods have been published to quantify irinotecan, SN-38 and other metabolites. Because of the availability of HPLC, LC-MS and LC-MS/MS methods, the pharmacokinetic profiling of irinotecan and its metabolites has been accomplished in multiple species, including cancer patients. The developed assays continue to find use in the optimization of newly designed delivery systems with regard to pharmacokinetics to promote safe and effective use of either irinotecan or SN-38. This review intends to: firstly, provide an exhaustive compilation of the published assays for irinotecan, SN-38 and other metabolite(s) of irinotecan, as applicable; secondly, to enumerate the validation parameters and applicable conclusions; and thirdly, provide some recent perspectives in the clinical pharmacology arena pertaining to efflux transporters, pediatric profiling, role of kidney function in defining toxicity, drug,drug interaction potential of irinotecan, etc. Copyright © 2009 John Wiley & Sons, Ltd. [source] | ||||||||||