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Determination of nicotine, cotinine, and related alkaloids in human urine and saliva by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.
J Pharm Biomed Anal. 2009 Jan 15; 49(1):108-14.JP

Abstract

A simple, rapid and sensitive method for the determination of nicotine, cotinine, nornicotine, anabasine, and anatabine in human urine and saliva was developed. These compounds were analyzed by on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Nicotine, cotinine and related alkaloids were separated within 7 min by high performance liquid chromatography (HPLC) using a Synergi 4u POLAR-RP 80A column and 5 mM ammonium formate/methanol (55/45, v/v) as a mobile phase at a flow-rate of 0.8 mL/min. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of these compounds. The optimum in-tube SPME conditions were 25 draw/eject cycles with a sample size of 40 microL using a CP-Pora PLOT amine capillary column as the extraction device. The extracted compounds could be desorbed easily from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS method, the calibration curves were linear in the concentration range of 0.5-20 ng/mL of nicotine, cotinine and related compounds in urine and saliva, and the detection limits (S/N=3) were 15-40 pg/mL. The method described here showed 20-46-fold higher sensitivity than the direct injection method (5 microL injection). The within-run and between-day precision (relative standard deviations) were below 4.7% and 11.3% (n=5), respectively. This method was applied successfully to analysis of urine and saliva samples without interference peaks. The recoveries of nicotine, cotinine and related compounds spiked into urine and saliva samples were above 83%, and the relative standard deviations were below 7.1%. This method was used to analyze urinary and salivary levels of these compounds in nicotine intake and smoking.

Authors+Show Affiliations

School of Pharmacy, Shujitsu University, Nishigawara, Okayama 703-8516, Japan. hkataoka@shujitsu.ac.jpNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19004590

Citation

Kataoka, Hiroyuki, et al. "Determination of Nicotine, Cotinine, and Related Alkaloids in Human Urine and Saliva By Automated In-tube Solid-phase Microextraction Coupled With Liquid Chromatography-mass Spectrometry." Journal of Pharmaceutical and Biomedical Analysis, vol. 49, no. 1, 2009, pp. 108-14.
Kataoka H, Inoue R, Yagi K, et al. Determination of nicotine, cotinine, and related alkaloids in human urine and saliva by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. J Pharm Biomed Anal. 2009;49(1):108-14.
Kataoka, H., Inoue, R., Yagi, K., & Saito, K. (2009). Determination of nicotine, cotinine, and related alkaloids in human urine and saliva by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. Journal of Pharmaceutical and Biomedical Analysis, 49(1), 108-14. https://doi.org/10.1016/j.jpba.2008.09.044
Kataoka H, et al. Determination of Nicotine, Cotinine, and Related Alkaloids in Human Urine and Saliva By Automated In-tube Solid-phase Microextraction Coupled With Liquid Chromatography-mass Spectrometry. J Pharm Biomed Anal. 2009 Jan 15;49(1):108-14. PubMed PMID: 19004590.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of nicotine, cotinine, and related alkaloids in human urine and saliva by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. AU - Kataoka,Hiroyuki, AU - Inoue,Reiko, AU - Yagi,Katsuharu, AU - Saito,Keita, Y1 - 2008/10/08/ PY - 2008/08/21/received PY - 2008/09/20/revised PY - 2008/09/25/accepted PY - 2008/11/14/pubmed PY - 2009/4/3/medline PY - 2008/11/14/entrez SP - 108 EP - 14 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 49 IS - 1 N2 - A simple, rapid and sensitive method for the determination of nicotine, cotinine, nornicotine, anabasine, and anatabine in human urine and saliva was developed. These compounds were analyzed by on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Nicotine, cotinine and related alkaloids were separated within 7 min by high performance liquid chromatography (HPLC) using a Synergi 4u POLAR-RP 80A column and 5 mM ammonium formate/methanol (55/45, v/v) as a mobile phase at a flow-rate of 0.8 mL/min. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of these compounds. The optimum in-tube SPME conditions were 25 draw/eject cycles with a sample size of 40 microL using a CP-Pora PLOT amine capillary column as the extraction device. The extracted compounds could be desorbed easily from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS method, the calibration curves were linear in the concentration range of 0.5-20 ng/mL of nicotine, cotinine and related compounds in urine and saliva, and the detection limits (S/N=3) were 15-40 pg/mL. The method described here showed 20-46-fold higher sensitivity than the direct injection method (5 microL injection). The within-run and between-day precision (relative standard deviations) were below 4.7% and 11.3% (n=5), respectively. This method was applied successfully to analysis of urine and saliva samples without interference peaks. The recoveries of nicotine, cotinine and related compounds spiked into urine and saliva samples were above 83%, and the relative standard deviations were below 7.1%. This method was used to analyze urinary and salivary levels of these compounds in nicotine intake and smoking. SN - 0731-7085 UR - https://www.unboundmedicine.com/medline/citation/19004590/Determination_of_nicotine_cotinine_and_related_alkaloids_in_human_urine_and_saliva_by_automated_in_tube_solid_phase_microextraction_coupled_with_liquid_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(08)00549-9 DB - PRIME DP - Unbound Medicine ER -