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DissertationDOI

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-
About: The article was published on 2006-01-01 and is currently open access. It has received 1 citations till now.

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Citations
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Journal Article
TL;DR: In this paper, a method was proposed for the determination of nicotine and cotinine in human urine, plasma and saliva, and the results showed that through the accurate determination of cotinines in saliva, the risk of ETS-exposed human can be predicted.

104 citations

References
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Journal ArticleDOI
TL;DR: A method for simultaneous determination of mecamylamine, nicotine, and the nicotine metabolite, cotinine, in human plasma using gas chromatography-mass spectrometry (GC-MS) is described.

51 citations

Journal ArticleDOI
TL;DR: The HPLC-ISP-MS method shows a good linearity over a concentration range from 5 to 200 ng/ml, making the method convenient for both clinical and forensic purposes.

48 citations

Journal ArticleDOI
TL;DR: The validated LC/MS assay proved to be appropriate for quantification of OX and DOX in plasma for clinical toxicology and therapeutic drug monitoring purposes and was found to be selective.
Abstract: Oxcarbazepine (OX), a new antiepileptic, may lead to unwanted side-effects or even life-threatening intoxications after overdose. Therefore, a validated liquid chromatographic/mass spectrometric (LC/MS) assay was developed for the quantification of OX and its pharmacologically active dihydro metabolite (dihydrooxcarbazepine, DOX, often named 10-hydroxycarbazepine). OX and DOX were extracted from plasma by the authors' standard liquid/liquid extraction and were separated on a Merck LiChroCART column with Superspher 60 RP Select B as the stationary phase. Gradient elution was performed using aqueous ammonium formate and acetonitrile. The compounds were quantified in the selected-ion monitoring mode using atmospheric pressure chemical ionization electrospray LC/MS. The assay was fully validated. It was found to be selective. The calibration curves were linear from 0.1 to 50 mg l(-1) for OX and DOX. Limits of quantification were 0.1 mg l(-1) for OX and DOX. The absolute recoveries were between 60 and 86%. The accuracy and precision data were within the required limits. The analytes in frozen plasma samples were stable for at least 1 month. The method was successfully applied to several authentic plasma samples from patients treated or intoxicated with OX. The measured therapeutic plasma levels ranged from 1 to 2 mg l(-1) for OX and from 10 to 40 mg l(-1) for DOX. The validated LC/MS assay proved to be appropriate for quantification of OX and DOX in plasma for clinical toxicology and therapeutic drug monitoring purposes. The assay is part of a general analysis procedure for the isolation, separation and quantification of various drugs and for their full-scan screening and identification.

47 citations

Journal ArticleDOI
TL;DR: The proposed LC-ESI-MS method was applied to measure the concentrations of nicotine and cotinine in hair of smokers and non-smokers to evaluate their self-reported smoking and exposure to environmental tobacco smoke and provided good selectivity, accuracy and precision.
Abstract: A simple liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method for the determination of nicotine and cotinine in human hair was established. In the procedure, a hair sample (10 mg) was washed with dichloromethane and digested in 2.5 M sodium hydroxide. The digest was extracted with dichloromethane and then 25 mM hydrochloric acid in methanol was added to the extract, to prevent loss of analytes. The solution was evaporated and redissolved in the mobile phase, methanol/10 mM ammonium acetate (30/70, v/v). A 20 microL aliquot of redissolved solution was subjected to analysis. Nicotine and cotinine in human hair were quantified by using deuterated analytes as internal standards. The quantification limits were 8 microg/L for nicotine and 0.9 microg/L for cotinine. The proposed method was applied to measure the concentrations of nicotine and cotinine in hair of smokers and non-smokers to evaluate their self-reported smoking and exposure to environmental tobacco smoke. In both cases, the method provided good selectivity, accuracy and precision.

47 citations

Journal ArticleDOI
TL;DR: A very sensitive and specific method was developed for the determination of aconitine, the main toxic alkaloid from plants of the genus Aconitum L., in biological samples and in two fatal cases with suspected aconite intoxication, ac onitine could be detected in blood samples at concentrations of 10.0 and 12.1 ng/g.
Abstract: A very sensitive and specific method was developed for the determination of aconitine, the main toxic alkaloid from plants of the genus Aconitum L., in biological samples. The method comprised solid-phase extraction using mixed-mode C8 cation exchange columns followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS). Chromatographic separation was achieved with a RP8 column. Detection of aconitine was achieved using electrospray in the positive ionisation mode and quantification was performed using multiple reaction monitoring with m/z 646.4 as precursor ion, i.e. [M+H]+ of aconitine and m/z 586.5, m/z 526.4 and m/z 368.4 as product ions after collision-induced dissociation. The method was fully validated for the analysis of blood samples: the limit of detection and the limit of quantitation were 0.1 ng/g and 0.5 ng/g, respectively. Within the linear calibration range of 0.5–25 ng/g, analytical recovery was 79.9%. In two fatal cases with suspected aconite intoxication, aconitine could be detected in blood samples at concentrations of 10.0 and 12.1 ng/g. In one case, aconitine could also be detected in the stomach content (3 ng/g) and in the other in the urine (180 ng/ml).

46 citations