Analysis of Succinylcholine in Tissues and Body Fluids by Ion-Pair Extraction and Gas Chromatography-Mass Spectrometry

Nordgren, Ingrid; Forney, Robert B.; Carroll, Frances; Holmstedt, Bo; Jäderholm-Ek, I; Pettersson, B.

doi:10.1007/978-3-642-69083-9_63

Cited by 18 publications

(9 citation statements)

References 7 publications

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“…Although far from being routine analysis, there exists a small number of previously published extraction methods for the parent drug, including protein precipitation1, 5 as well as solid‐phase extraction (SPE) schemes using C 1 ‐,6, 7 C 18 ‐12 and carboxylic acid (CBA)11‐cartridges. Liquid–liquid extraction (LLE) has equally been applied for sample clean‐up, the necessary ion‐pairing reagents being hexanitrodiphenylamine (DPA)13–15 or potassium triiodide (KI 3 ) 16. LeBeau et al 8 as well as Ballard et al 9 further reported a rather complex SUX extraction procedure, consisting of an LLE step in combination with reverse‐phase ion‐pairing SPE using heptafluorobutyric acid (HFBA) as the ion‐pairing reagent.…”

Section: Introductionmentioning

confidence: 99%

A fully validated isotope dilution HPLC‐MS/MS method for the simultaneous determination of succinylcholine and succinylmonocholine in serum and urine samples

2008

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A high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) method for the simultaneous detection of succinylcholine (SUX) and its metabolite succinylmonocholine (SMC) in serum and urine is presented. For internal standardization using isotope dilution, the deuterated compounds SUX-d(18) and SMC-d(3) were employed. Full validation was performed according to international guidelines. Solid-phase extraction (SPE) of acidified samples was accomplished using Strata-X polymeric reversed phase cartridges together with heptafluorobutyric acid (HFBA) as ion-pairing reagent. Separation was achieved within 13 min on a Phenomenex Synergi Hydro RP C18 column (4 microm, 150 x 2 mm) using a gradient of 5 mM ammonium formate buffer pH 3.5 and acetonitrile.To ensure the method's applicability in forensic as well as clinical toxicology, the specific demands of both research fields were taken into account, and the method was thus validated for a low and high concentration range. For both serum and urine as sample matrix, the validation revealed good intraday and interday precisions, consistently ranging below 15% for the lowest and below 10% for elevated concentrations. Accuracy was likewise good and never exceeded 10%. Extraction recovery was excellent, ranging between 88.1 and 103.9% for SUX and SMC in both tested matrices. Matrix effects were significant, the otherwise optimized extraction and detection methods, however, allowed for a very satisfactory sensitivity of the described method: For serum, the limits of detection and quantitation were determined to be 1.9 and 6.0 ng/ml for SUX, as well as 2.5 and 8.6 ng/ml for SMC, respectively; for urine, the corresponding values were established to be 1.4 and 4.0 ng/ml (SUX), as well as 1.5 and 4.9 ng/ml (SMC).The presented method was successfully applied to authentic samples of two forensic cases investigated in the institute of forensic medicine in Bonn, allowing the diagnosis of SUX intoxications.

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Section: Introductionmentioning

confidence: 99%

A fully validated isotope dilution HPLC‐MS/MS method for the simultaneous determination of succinylcholine and succinylmonocholine in serum and urine samples

2008

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“…More recent cases have prompted the development of a specific and sensitive chemical method to be used forensically as well as clinically. The method is based upon gas chromatography -mass spectrometry and deuterium labelled internal standard (Nordgren et al, 1983). It is now possible to analyze concentrations of SCh as low as 2 ng/g tissue.…”

Section: Discussionmentioning

confidence: 99%

Neurobiology of Acetylcholine

Dun¹,

Perlman²,

Karczmar³

1987

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“…However, target analyses for the detection of SUX and succinylmonocholine (SMC) according to previously published procedures using thin-layer chromatography [1], GC/MS [1,8,27] and liquid chromatography/mass spectrometry (LC/MS) [2,17,32] revealed negative results.…”

Section: Autopsy Findingsmentioning

confidence: 99%

Fall downstairs: accident, homicide or natural death?

Madea

Dettmeyer

Mußhoff

2007

Forensic Sci Med Pathol

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In homicide cases a clear anatomical or toxicological cause of death is normally evident. In the following a case is described where, without clear anatomical or toxicological cause of death, the husband of the deceased-a trained anaesthesiologist-was charged with murder. Suspicion was raised since the autopsy findings did not correspond to a fatal fall downstairs but instead could be definitely ruled out as cause of death, since intracranial bleedings and cerebral contusions, the leading causes of death in fatal falls downstairs, were missing. Further suspicion was raised since electrocardiograms (ECGs), previously stated by the accused to have been recorded personally from his wife during cardiopulmonary resuscitation (CPR), were obviously faked. Additionally, an ampule of succinylcholine was missing from his emergency case. In a trial lasting more than three quarters of a year with several witnesses and experts heard by the court, the cause of death remained unclear. However, a natural cause of death and a fatal fall downstairs were ruled out. Subsequently the husband admitted during the trial to have killed his wife without elaborating on the circumstances for legal reasons. He was sentenced to prolonged imprisonment. Of special importance was that, based on the knowledge of typical autopsy findings in fatal falls downstairs, a lethal fall downstairs could be ruled out. Therefore even negative autopsy findings are of great forensic importance.

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Analysis of Succinylcholine in Tissues and Body Fluids by Ion-Pair Extraction and Gas Chromatography-Mass Spectrometry

Cited by 18 publications

References 7 publications

A fully validated isotope dilution HPLC‐MS/MS method for the simultaneous determination of succinylcholine and succinylmonocholine in serum and urine samples

A fully validated isotope dilution HPLC‐MS/MS method for the simultaneous determination of succinylcholine and succinylmonocholine in serum and urine samples

Neurobiology of Acetylcholine

Fall downstairs: accident, homicide or natural death?

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