Abstract
A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic–mass spectrometric (GC–MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA), before GC–MS analysis. Linearity was good for Δ 9-tetrahydrocannabinol (THC), cannabidiol, and cannabinol; regression coefficients were greater than 0.99. Depending on the characteristics of the matrix the detection limits obtained ranged between 0.01 and 0.17 mg kg−1 and the precision between 0.4 and 11.8%. In comparison with conventional liquid–liquid extraction this automated HS-SPME–GC–MS procedure is substantially faster. It is easy to perform, solvent-free, and sample quantities are minimal, yet it maintains the same sensitivity and reproducibility. The applicability was demonstrated by analysis of 30 hemp food samples. Cannabinoids were detected in all of the samples and it was possible to differentiate between drug-type and fiber-type Cannabis sativa L. In comparison with other studies relatively low THC concentrations between 0.01 and 15.53 mg kg−1 were determined.
Similar content being viewed by others
References
Turner CE, Elsohly MA, Boeren EG (1980) J Nat Prod 43:169–234
Fetterman PS, Keith ES, Waller CW, Guerrero O, Doorenbos NJ, Quimby MW (1971) J Pharm Sci 60:1246–1249
Avico U, Pacifici R, Zuccaro P (1985) Bull Narc 37:61–65
de Meijer EPM, van der Kamp HJ, van Eeuwijk FA (1992) Euphytica 62:187–200
Alt A, Reinhardt G (1996) Blutalkohol 33:347–356
Costantino A, Schwartz RH, Kaplan P (1997) J Anal Toxicol 21:482–485
Callaway JC, Weeks RA, Raymon LP, Walls HC, Hearn WL (1997) J Anal Toxicol 21:319–320
Struempler RE, Nelson G, Urry FM (1997) J Anal Toxicol 21:283–285
Lehmann T, Sager F, Brenneisen R (1997) J Anal Toxicol 21:373–375
Alt A, Reinhardt G (1998) J Anal Toxicol 22:80–81
Giroud C, Augsburger M, Rivier L, Mangin P (1997) Hemp tea versus hemp milk: subjective effects and elimination studies of THC and its main metabolite. In: Proc 35th TIAFT Meeting, Padova, Italy, pp 112–121
Alt A (1997) Lebensmittel auf Hanfbasis und deren forensische Bedeutung. In: GTFCh-Symposium 1997. Verlag Dr Helm, Heppenheim, Germany, pp 156–165
Meier H, Vonesch HJ (1997) Schweiz Med Wochenschr 127:214–218
Mölleken H (1999) Bioforum 7/8:452–457
Leizer C, Ribnicky D, Poulev A, Dushenkov S, Raskin I (2000) J Nutraceut Funct Med Foods 2:35–53
European Council (1998) Off J Eur Comm L190:7–8
Mediavilla V, Derungs R, Känzig A, Mägert A (1997) Agrarforschung 4:449–451
BgVV (1997) Einsatz von Hanf in Lebensmitteln kann gesundheitlich problematisch sein. BgVV Pressedienst, Berlin, Germany
BgVV (2000) BgVV empfiehlt Richtwerte für THC (Tetrahydrocannabinol) in hanfhaltigen Lebensmitteln. BgVV Pressedienst, Berlin, Germany
Bosy TZ, Cole KA (2000) J Anal Toxicol 24:562–566
Zoller O, Rhyn P, Zimmerli B (2000) J Chromatogr A 872:101–110
Iten PX, Coray M (1996) Hanf-Bier neu auf dem Markt in der Schweiz—THC-Gehalt und forensische Bedeutung. 75. Jahrestagung der Deutschen Gesellschaft für Rechtsmedizin. Zürich, Switzerland
Alt A, Reinhardt G (1997) Blutalkohol 34:286–293
Ross SA, Mehmedic Z, Murphy TP, Elsohly MA (2000) J Anal Toxicol 24:715–717
Gibson CR, Williams RD, Browder RO (1998) J Anal Toxicol 22:179
Amtliche Sammlung von Untersuchungsverfahren nach §35 LMBG (2000) L13.04.19–1:1–2
Boess C, Palavinskas B, Dusemund B, Gebhardt G, Blaas W (2000) Lebensmittelchemie 54:104–105
Georgi K, Mavric E, Speer K (2002) Dtsch Lebensm Rdsch 98:363–366
Matsunaga T, Nagatomo H, Yamamoto I, Yoshimura H (1990) Esei Kagaku 36:545–547
Grassi G (1999) J Int Hemp Assoc 6:63–66
European Commission (1999) Community method for the quantitative determination of Δ 9-THC (Tetrahydrocannabinol) content in hemp varieties. In: Commission Regulation (EC) No 2316/1999 laying down detailed rules for the application of Council Regulation (EC) No 1251/1999 establishing a support system for producers of certain arable crops. Off J Eur Comm L280:43–65
Arthur CL, Pawliszyn J (1990) Anal Chem 62:2145–2148
Kataoka H, Lord HL, Pawliszyn J (2000) J Chromatogr A 880:35–62
Hall BJ, Satterfield-Doerr M, Parikh AR, Brodbelt JS (1998) Anal Chem 70:1788–1796
Strano-Rossi S, Chiarotti M (1999) J Anal Toxicol 23:7–10
Sporkert F, Pragst F (2000) Forensic Sci Int 107:129–148
Musshoff F, Junker HP, Lachenmeier DW, Kroener L, Madea B (2002) J Anal Toxicol 26:554–560
Meier PC, Zünd RE (2000), Statistical methods in analytical chemistry. Wiley, New York, USA
DIN 32 645 (1994), Chemische Analytik: Nachweis-, Erfassungs- und Bestimmungsgrenze, Ermittlung unter Wiederholbedingungen. Begriffe, Verfahren, Auswertung. Beuth Verlag, Berlin, Germany
Page BD, Lacroix G (1993) J Chromatogr 648:199–211
Forsyth DS, Dusseault L (1997) Food Addit Contam 14:301–307
Lachenmeier DW, Kröner L, Mußhoff F, Madea B (2003) Lebensmittelchemie 57:76
Lachenmeier DW, Kroener L, Musshoff F, Madea B (2003) Rapid Commun Mass Spectrom 17:472–478
Musshoff F, Lachenmeier DW, Kroener L, Madea B (2003) Forensic Sci Int 133:32–38
Fortner N, Fogerson R, Lindman D, Iversen T, Armbruster D (1997) J Anal Toxicol 21:476–481
Kunsman GW, Kunsman CM, Levine B, Smith ML (1999) J Anal Toxicol 23:563–564
Leson G, Pless P, Grotenhermen F, Kalant H, Elsohly MA (2001) J Anal Toxicol 25:691–698
Cirimele V, Kintz P, Jamey C, Ludes B (1999) J Anal Toxicol 23:349–351
Alt A, Reinhardt G (1997) Z Verkehrssicherheit 43:74–77
Alt A, Bräutigam A, Reinhardt G (1998) Z Verkehrssicherheit 44:33–35
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Lachenmeier, D.W., Kroener, L., Musshoff, F. et al. Determination of cannabinoids in hemp food products by use of headspace solid-phase microextraction and gas chromatography–mass spectrometry. Anal Bioanal Chem 378, 183–189 (2004). https://doi.org/10.1007/s00216-003-2268-4
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-003-2268-4