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Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case.

Mannocchi G, Pantano F, Tittarelli R, Catanese M, Umani Ronchi F, Busardò FP - Int J Anal Chem (2015)

Bottom Line: Methadone-d9 was used as internal standard.Results.Conclusions.

View Article: PubMed Central - PubMed

Affiliation: Department of Anatomical, Histological, Forensic and Orthopaedic Sciences, Sapienza University of Rome, Viale Regina Elena 336, 00161 Rome, Italy.

ABSTRACT
Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug. Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS). Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE) technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v) and analysis was followed by GC-MS. Methadone-d9 was used as internal standard. Results. The limit of detection (LOD) was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ) was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively. Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case.

No MeSH data available.


Internal examination: overdistended bladder containing 3.7 L of urine.
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Related In: Results  -  Collection


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fig2: Internal examination: overdistended bladder containing 3.7 L of urine.

Mentions: The external examination revealed only a remarkable abdominal swelling. The internal examination showed a moderate pulmonary oedema and the presence of massive urinary retention: the bladder contained 3.7 L of urine (Figure 2). The kidneys (weight 270 gr, the right, and 260 gr, the left) were markedly congested.


Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case.

Mannocchi G, Pantano F, Tittarelli R, Catanese M, Umani Ronchi F, Busardò FP - Int J Anal Chem (2015)

Internal examination: overdistended bladder containing 3.7 L of urine.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4508480&req=5

fig2: Internal examination: overdistended bladder containing 3.7 L of urine.
Mentions: The external examination revealed only a remarkable abdominal swelling. The internal examination showed a moderate pulmonary oedema and the presence of massive urinary retention: the bladder contained 3.7 L of urine (Figure 2). The kidneys (weight 270 gr, the right, and 260 gr, the left) were markedly congested.

Bottom Line: Methadone-d9 was used as internal standard.Results.Conclusions.

View Article: PubMed Central - PubMed

Affiliation: Department of Anatomical, Histological, Forensic and Orthopaedic Sciences, Sapienza University of Rome, Viale Regina Elena 336, 00161 Rome, Italy.

ABSTRACT
Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug. Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS). Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE) technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v) and analysis was followed by GC-MS. Methadone-d9 was used as internal standard. Results. The limit of detection (LOD) was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ) was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively. Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case.

No MeSH data available.