LC-MS determination of Taxus alkaloids in biological specimens

Beike, Justus; Karger, B.; Meiners, T.; Brinkmann, B.; Köhler, Helga

doi:10.1007/s00414-003-0399-y

Cited by 37 publications

(36 citation statements)

References 18 publications

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“…These substances need to be hydrolysed and/or derivatised to be accessible with this technique. As an alternative, liquid chromatography coupled to mass spectrometry (LC-MS) is an upcoming routine method in laboratories involved in analytical toxicology [1][2][3][4]. With LC-MS-MS, an unequivocal identification of many compounds can be carried out without previous hydrolysis and derivatisation.…”

Section: Introductionmentioning

confidence: 99%

Quantification of benzodiazepines in whole blood and serum

Dussy¹,

Hamberg²,

Briellmann³

2005

Int J Legal Med

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A high-performance liquid chromatography method for the determination of benzodiazepines and their metabolites in whole blood and serum using mass spectrometry (MS) and photodiode array (PDA) detection is presented. The combination of both detection types can complement each other and provides extensive case relevant data. The limits of quantification (LOQ) with the MS detection lie between 2 and 3 microg/l for the following benzodiazepines or metabolites: 7-amino-flunitrazepam, alprazolam, desalkyl-flurazepam, desmethyl-flunitrazepam, diazepam, flunitrazepam, flurazepam, alpha-hydroxy-midazolam, lorazepam, midazolam, nitrazepam, nordazepam and oxazepam, respectively 5 microg/l for lormetazepam and 6 microg/l for bromazepam. The LOQ of clobazam determined with the PDA detector is 10 microg/l. A convenient approach for determining the measurement uncertainty of the presented method--applicable also for other methods in an accreditation process--is presented. At low concentrations (<10 microg/l), measurement uncertainty was estimated to be about 50%, and at concentrations >180 microg/l, it was estimated to be about 15%. One hundred and twenty-eight case data acquired over 1 year are summarised.

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Section: Introductionmentioning

confidence: 99%

Quantification of benzodiazepines in whole blood and serum

Dussy¹,

Hamberg²,

Briellmann³

2005

Int J Legal Med

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“…In the past, liquid chromatography-mass spectrometry (LC-MS) has been successfully applied for the analysis of other toxic plant ingredients [24]. For the determination of aconitine-type alkaloids in particular, a variety of analytical techniques have been used.…”

Section: Introductionmentioning

confidence: 99%

Determination of aconitine in body fluids by LC-MS-MS

et al. 2004

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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 Cs 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).

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“…Ingestions of needles or yew decoctions for suicidal purposes have been reported. Accidental ingestions repeatedly occur with children eating the red aril including the seeds [1,[4][5][6][7][8][9][10].…”

Section: Introductionmentioning

confidence: 99%

“…However, there are known cases where plant material was already degraded in the stomach or not present at all because a decoction of yew has been ingested [9,14]. In these cases, determination of taxine in biological samples is essential.…”

Section: Introductionmentioning

confidence: 99%

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Quantitative determination of taxine B in body fluids by LC–MS–MS

Frommherz

Kintz²,

Kijewski³

et al. 2006

Int J Legal Med

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A new specific and sensitive LC-MS-MS method for the detection of taxine B and isotaxine B, the main toxic pseudo-alkaloids from yew (Taxus sp.), in biological samples (blood, urine, gastric content) was developed. Biological samples were prepared for LC-MS-MS by means of solid-phase extraction (SPE) procedure and yielded a recovery of 86%. Chromatographic separation was achieved using an RP(18) column. Detection of taxine B and isotaxine B was performed using multiple reaction monitoring with m/z 584.2 as precursor ion, i.e. [M+H](+), of both isomers and m/z 194.3 and m/z 107.1 as product ions after collision-induced dissociation. Docetaxel was applied as internal standard. The method was fully validated for the analysis of blood samples. Linearity was proven in the range from 0.1-500 ng/g. The limit of detection and the limit of quantitation are 0.4 and 2 ng/g, respectively. The method was applied to the determination of taxine B and isotaxine B in four fatal cases (two humans, two horses) with suspected yew intoxication. Blood levels were 105, 168, 174 and 212 ng/g.

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LC-MS determination of Taxus alkaloids in biological specimens

Cited by 37 publications

References 18 publications

Quantification of benzodiazepines in whole blood and serum

Quantification of benzodiazepines in whole blood and serum

Determination of aconitine in body fluids by LC-MS-MS

Quantitative determination of taxine B in body fluids by LC–MS–MS

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