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Validation of a SPE-LC-MS/MS method for the determination of ketamine and norketamine in micropulverized hair after a single IV dose.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Oct 15; 1033-1034:200-209.JC

Abstract

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.

Authors+Show Affiliations

Instituto de Química, Universidade Federal Fluminense, Outeiro de S. João Batista S/N, Niterói, RJ, Brazil.Instituto de Química, Universidade Federal Fluminense, Outeiro de S. João Batista S/N, Niterói, RJ, Brazil.LaboratórioToxFree, Faculdade de Farmácia, Universidade Federal Fluminense, Rua Mário Viana, 523, Santa Rosa, Niterói, RJ, Brazil.Instituto de Química, Universidade Federal Fluminense, Outeiro de S. João Batista S/N, Niterói, RJ, Brazil. Electronic address: silvanavr@id.uff.br.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

27567376

Citation

Barreto, Adriana S., et al. "Validation of a SPE-LC-MS/MS Method for the Determination of Ketamine and Norketamine in Micropulverized Hair After a Single IV Dose." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1033-1034, 2016, pp. 200-209.
Barreto AS, Brant VF, Spinelli E, et al. Validation of a SPE-LC-MS/MS method for the determination of ketamine and norketamine in micropulverized hair after a single IV dose. J Chromatogr B Analyt Technol Biomed Life Sci. 2016;1033-1034:200-209.
Barreto, A. S., Brant, V. F., Spinelli, E., & Rodrigues, S. V. (2016). Validation of a SPE-LC-MS/MS method for the determination of ketamine and norketamine in micropulverized hair after a single IV dose. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1033-1034, 200-209. https://doi.org/10.1016/j.jchromb.2016.08.027
Barreto AS, et al. Validation of a SPE-LC-MS/MS Method for the Determination of Ketamine and Norketamine in Micropulverized Hair After a Single IV Dose. J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Oct 15;1033-1034:200-209. PubMed PMID: 27567376.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Validation of a SPE-LC-MS/MS method for the determination of ketamine and norketamine in micropulverized hair after a single IV dose. AU - Barreto,Adriana S, AU - Brant,Vinnicius F, AU - Spinelli,Eliani, AU - Rodrigues,Silvana V, Y1 - 2016/08/17/ PY - 2016/05/31/received PY - 2016/08/10/revised PY - 2016/08/16/accepted PY - 2016/8/28/entrez PY - 2016/8/28/pubmed PY - 2017/2/18/medline KW - Extraction KW - Hair analysis KW - Ketamine KW - LC–MS/MS KW - Norketamine SP - 200 EP - 209 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1033-1034 N2 - 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. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/27567376/Validation_of_a_SPE_LC_MS/MS_method_for_the_determination_of_ketamine_and_norketamine_in_micropulverized_hair_after_a_single_IV_dose_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30639-0 DB - PRIME DP - Unbound Medicine ER -