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Development of procedures for sreening for, identification and/or validated quantification of herbal drugs in blood or urine using GC-MS, LC-MS or LC-MS/MS

01 Jan 2006-

AboutThe article was published on 2006-01-01 and is currently open access. It has received 1 citation(s) till now. more

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Abstract: A method is proposed for the determination of nicotine and cotinine in human urine, plasma and saliva. Nicotine and cotinine were extracted from alkalinized sample with ethyl ether and concentrated to minimum volume with nitrogen stream. The volatility of nicotine was prevented by the addition of acetic acid to the organic solvent during evaporation. Peak shapes and quantitation of nicotine and cotinine are excellent, with linear calibration curves over a wide range of 1-10 000 ng/ml. The detection limits of nicotine and cotinine are 0.2 ng/ml in urine and 1.0 ng/ml in plasma and saliva. The intra-day precision of nicotine and cotinine in all samples was <5% relative standard deviation (RSD). Urine, plasma and saliva samples of 303 non-smoking and 41 smoking volunteers from a girl's high school in Korea were quantified by the described procedure. As a result, the concentrations of nicotine and cotinine in plasma ranged from 6 to 498 ng/ml and 4 to 96 ng/ml. Otherwise, those of nicotine and cotinine in saliva ranged from 0 to 207 ng/ml and 0 to 42 ng/ml, and those of nicotine and cotinine in urine ranged from 0 to 1590 ng/ml and 0 to 2986 ng/ml, respectively. We found that the concentration of cotinine in plasma was successfully predicted from the salivary cotinine concentration by the equation y=2.31x+4.76 (x=the concentration of cotinine in saliva, y=the concentration of cotinine in plasma). The results show that through the accurate determination of cotinine in saliva, the risk of ETS-exposed human can be predicted.

104 citations

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TL;DR: Practical, experimental approaches for studying, identifying, and eliminating the effect of matrix on the results of quantitative analyses by HPLC-MS/MS are described and it is demonstrated that, for the investigational drug under study, the matrix effect was clearly observed when ISP interface was utilized but it was absent when the HN interface was employed.
Abstract: In recent years, high-performance liquid chromatography (HPLC) with tandem mass spectrometric (MS/MS) detection has been demonstrated to be a powerful technique for the quantitative determination of drugs and metabolites in biological fluids. However, the common and early perception that utilization of HPLC−MS/MS practically guarantees selectivity is being challenged by a number of reported examples of lack of selectivity due to ion suppression or enhancement caused by the sample matrix and interferences from metabolites. In light of these serious method liabilities, questions about how to develop and validate reliable HPLC−MS/MS methods, especially for supporting long-term human pharmacokinetic studies, are being raised. The central issue is what experiments, in addition to the validation data usually provided for the conventional bioanalytical methods, need to be conducted to confirm HPLC−MS/MS assay selectivity and reliability. The current regulatory requirements include the need for the assessment and...

4,123 citations

01 Jan 1966
Abstract: 1. Introduction 2. Elemental Composition 3. The Molecular Ion 4. Basic Mechanisms of Ion Fragmentation 5. Postulation of Molecular Structures 6. Auxiliary Techniques 7. Theory of Unimolecular Ion Decompositions 8. Detailed Mechanisms of Ion Fragmentation 9. Mass Spectra of Common Compound Classes 10.Computer Identification of Unknown Mass Spectra 11.Solutions to Unknowns Bibliography Appendix Index

2,069 citations

Journal ArticleDOI
Abstract: For the characterization of organic substances in gas chromatography a number termed «retention index» is proposed. A simple relation exists between the retention index of a compound on a non-polar stationary phase and its boiling point.

1,820 citations

Journal ArticleDOI
TL;DR: The purpose of this report is to represent the progress in analytical methodologies over the last decade and assessment of the major agreements and issues discussed with regard to small molecules at both the conference and the workshop.
Abstract: This report is a synthesis of (1) the earlier conference on Analytical Methods Validation−Bioavailability, Bioequivalence and Pharmacokinetic Studies (Conference held in Arlington, VA, December 3–5, 1990 and the report published in Pharmaceutical Research, 9: 588-592, 1992) and (2) the workshop on “Bioanalytical Methods Validation—A Revisit with a Decade of Progress,” (Workshop held in Arlington, VA, January 12–14, 2000), sponsored by the American Association of Pharmaceutical Scientists and the U. S. Food and Drug Administration. The bioanalytical method validation workshop of January 12–14, 2000 was directed towards small molecules. A separate workshop was held in March 1–3, 2000 to discuss validation principles for macromolecules. The purpose of this report is to represent the progress in analytical methodologies over the last decade and assessment of the major agreements and issues discussed with regard to small molecules at both the conference and the workshop. The report is also intended to provide guiding principles for validation of bioanalytical methods employed in support of bioavailability, bioequivalence, and pharmacokinetic studies in man and in animals.

1,560 citations

Journal ArticleDOI
TL;DR: Important considerations in analytical method validation will be discussed and may be used as guidance by scientists wishing to develop and validate analytical methods.
Abstract: Reliable analytical data are a prerequisite for correct interpretation of toxicological findings in the evaluation of scientific studies, as well as in daily routine work. Unreliable analytical data might not only be contested in court, but could also lead to unjustified legal consequences for the defendant or to wrong treatment of the patient. Therefore, new analytical methods to be used in forensic and/or clinical toxicology require careful method development and thorough validation of the final method. This is especially true in the context of quality management and accreditation, which have become matters of increasing relevance in analytical toxicology in recent years. In this paper, important considerations in analytical method validation will be discussed which may be used as guidance by scientists wishing to develop and validate analytical methods.

1,051 citations