Validation of a SPE-LC–MS/MS method for the determination of ketamine and norketamine in micropulverized hair after a single IV dose
| Autor: | Silvana Vianna Rodrigues, Eliani Spinelli, Vinnicius F. Brant, Adriana da Silva Barreto |
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| Rok vydání: | 2016 |
| Předmět: |
Adult
Clinical Biochemistry 01 natural sciences Biochemistry Analytical Chemistry 03 medical and health sciences 0302 clinical medicine Limit of Detection Tandem Mass Spectrometry Norketamine medicine Humans Ketamine 030216 legal & forensic medicine Solid phase extraction Aged Chromatography Dose-Response Relationship Drug Chemistry Solid Phase Extraction 010401 analytical chemistry Hair analysis Extraction (chemistry) Phosphate buffered saline Reproducibility of Results Cell Biology General Medicine Surgical procedures Spe lc ms ms 0104 chemical sciences Calibration Injections Intravenous Female Chromatography Liquid Hair medicine.drug |
| Zdroj: | Journal of Chromatography B. :200-209 |
| ISSN: | 1570-0232 |
| Popis: | A SPE-LC-MS/MS method for the determination of ketamine (KET) and norketamine (NKET) was developed and validated. Extensive pulverization (25min at 25Hz) of previously cooled samples (5min in liquid nitrogen) allowed for extraction in a phosphate buffer (pH 6) solution after 10min vortex agitation at room temperature, simplifying the coupling of the extraction to an effective mixed-mode SPE (solid phase extraction) clean-up procedure. The extraction optimization was performed with samples fortified by drug incorporation according to a published procedure involving incubation of blank matrices for 16days. The method was validated for selectivity, matrix effect, linearity, LLQ (lower limit of quantification), precision, accuracy, recovery, carryover and stability after preparation and has proven to be accurate and reliable within a range of 0.02-10ng/mg for KET and 0.04-4ng/mg for NKET, meeting proposed KET cutoffs for discrimination from chronic use. In addition, the method was sensitive enough to detect the drugs after unique small (1mg/kg) intravenous doses received by patients submitted to general anesthesia before surgical procedures. Ketamine levels varied from 0.060 to 0.111ng/mg and norketamine was positive (LLQ) in all samples. The high sensitivity achieved with conventional 3D-ion-trap MS/MS detection is probably due to the simple but very effective proposed procedure. |
| Databáze: | OpenAIRE |
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