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Detection and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair by GC/MS/MS in Negative Chemical Ionization mode (NCI) with a simple and rapid liquid/liquid extraction.
Forensic Sci Int. 2012 May 10; 218(1-3):49-52.FS

Abstract

INTRODUCTION

The fine detection of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in hair matrix remains one of the most important topics in hair analysis. This relevance lies in the necessity to obtain evidence of effective drug consumption and dispel any doubt of environmental contamination. THCCOOH is the highest and mainly represented Δ9-THC metabolite, but its concentration in hair is very low. A sensitive method for quantitative determination of THCCOOH in hair was developed. As first step, the method was tested with different SPE/LLE conditions, but the best results were obtained with a simple ad hoc LLE extraction. The final method was fully validated, evaluating parameters like extraction recovery, linearity, specificity and sensitivity. More than one hundred hair samples were then analyzed with the validated method. Data analysis was performed so as to determine respective concentrations of the metabolite and active molecule.

METHODS

Hair was washed and cut into small pieces (2-4mm). Samples (20-50mg) were spiked with deuterated internal standard (THC-d(3) and THCCOOH-d(3)) and then hydrolyzed at 90°C in 1mL of 1M NaOH for 15min. THC was isolated by a LLE basic extraction with n-hexane:ethyl acetate (9:1). Next the aqueous solution was acidified (pH 4) adding concentrated acetic acid. THCCOOH was extracted with the same mixture. Dried extracts were derivatized with pentafluoropropionic anhydride and hexafluoroisopropanol and analyzed by GC/MS/MS (Agilent 7000B triple quadrupole) in NCI mode.

RESULTS

The linear range of THCCOOH is 0.1-5pg/mg, with good correlation coefficients (r(2)>0.9993). This method has great sensitivity (LOD 0.01pg/mg to LOQ 0.04pg/mg), high recovery, reproducibility and robustness.

CONCLUSIONS

Based on these results, the method proved to be effective for the rapid determination of THC and THCCOOH in hair specimens.

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Authors+Show Affiliations

Minoli M
Section of Forensic Toxicology, Department of Human Physiology, University of Milan, Italy. mauro.minoli@unimi.it
Angeli I
No affiliation info available
Ravelli A
No affiliation info available
Gigli F
No affiliation info available
Lodi F
No affiliation info available

MeSH

DronabinolForensic ToxicologyGas Chromatography-Mass SpectrometryHairHallucinogensHumansLimit of DetectionSubstance Abuse Detection

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

22036308

Citation

Minoli, M, et al. "Detection and Quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic Acid in Hair By GC/MS/MS in Negative Chemical Ionization Mode (NCI) With a Simple and Rapid Liquid/liquid Extraction." Forensic Science International, vol. 218, no. 1-3, 2012, pp. 49-52.
Minoli M, Angeli I, Ravelli A, et al. Detection and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair by GC/MS/MS in Negative Chemical Ionization mode (NCI) with a simple and rapid liquid/liquid extraction. Forensic Sci Int. 2012;218(1-3):49-52.
Minoli, M., Angeli, I., Ravelli, A., Gigli, F., & Lodi, F. (2012). Detection and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair by GC/MS/MS in Negative Chemical Ionization mode (NCI) with a simple and rapid liquid/liquid extraction. Forensic Science International, 218(1-3), 49-52. https://doi.org/10.1016/j.forsciint.2011.10.014
Minoli M, et al. Detection and Quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic Acid in Hair By GC/MS/MS in Negative Chemical Ionization Mode (NCI) With a Simple and Rapid Liquid/liquid Extraction. Forensic Sci Int. 2012 May 10;218(1-3):49-52. PubMed PMID: 22036308.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Detection and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair by GC/MS/MS in Negative Chemical Ionization mode (NCI) with a simple and rapid liquid/liquid extraction. AU - Minoli,M, AU - Angeli,I, AU - Ravelli,A, AU - Gigli,F, AU - Lodi,F, Y1 - 2011/10/27/ PY - 2011/04/01/received PY - 2011/06/06/accepted PY - 2011/11/1/entrez PY - 2011/11/1/pubmed PY - 2012/9/26/medline SP - 49 EP - 52 JF - Forensic science international JO - Forensic Sci Int VL - 218 IS - 1-3 N2 - INTRODUCTION: The fine detection of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in hair matrix remains one of the most important topics in hair analysis. This relevance lies in the necessity to obtain evidence of effective drug consumption and dispel any doubt of environmental contamination. THCCOOH is the highest and mainly represented Δ9-THC metabolite, but its concentration in hair is very low. A sensitive method for quantitative determination of THCCOOH in hair was developed. As first step, the method was tested with different SPE/LLE conditions, but the best results were obtained with a simple ad hoc LLE extraction. The final method was fully validated, evaluating parameters like extraction recovery, linearity, specificity and sensitivity. More than one hundred hair samples were then analyzed with the validated method. Data analysis was performed so as to determine respective concentrations of the metabolite and active molecule. METHODS: Hair was washed and cut into small pieces (2-4mm). Samples (20-50mg) were spiked with deuterated internal standard (THC-d(3) and THCCOOH-d(3)) and then hydrolyzed at 90°C in 1mL of 1M NaOH for 15min. THC was isolated by a LLE basic extraction with n-hexane:ethyl acetate (9:1). Next the aqueous solution was acidified (pH 4) adding concentrated acetic acid. THCCOOH was extracted with the same mixture. Dried extracts were derivatized with pentafluoropropionic anhydride and hexafluoroisopropanol and analyzed by GC/MS/MS (Agilent 7000B triple quadrupole) in NCI mode. RESULTS: The linear range of THCCOOH is 0.1-5pg/mg, with good correlation coefficients (r(2)>0.9993). This method has great sensitivity (LOD 0.01pg/mg to LOQ 0.04pg/mg), high recovery, reproducibility and robustness. CONCLUSIONS: Based on these results, the method proved to be effective for the rapid determination of THC and THCCOOH in hair specimens. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/22036308/abstract/Detection_and_quantification_of_11_nor_Δ9_tetrahydrocannabinol_9_carboxylic_acid_in_hair_by_GC/MS/MS_in_Negative_Chemical_Ionization_mode__NCI__with_a_simple_and_rapid_liquid/liquid_extraction_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(11)00489-0 DB - PRIME DP - Unbound Medicine ER -
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