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Kumazawa T, Hasegawa C, Lee XP, et al. Pipette tip solid-phase extraction and gas chromatography-mass spectrometry for the determination of mequitazine in human plasma. Talanta. 2006;70(2):474-8doi: 10.1016/j.talanta.2006.02.059.
Kumazawa, T., Hasegawa, C., Lee, X. P., Marumo, A., Shimmen, N., Ishii, A., Seno, H., & Sato, K. (2006). Pipette tip solid-phase extraction and gas chromatography-mass spectrometry for the determination of mequitazine in human plasma. Talanta, 70(2), 474-8. https://doi.org/10.1016/j.talanta.2006.02.059
Kumazawa, Takeshi, et al. "Pipette tip solid-phase extraction and gas chromatography-mass spectrometry for the determination of mequitazine in human plasma." Talanta vol. 70,2 (2006): 474-8. doi: https://doi.org/10.1016/j.talanta.2006.02.059
Kumazawa T, Hasegawa C, Lee XP, Marumo A, Shimmen N, Ishii A, Seno H, Sato K. Pipette tip solid-phase extraction and gas chromatography-mass spectrometry for the determination of mequitazine in human plasma. Talanta. 2006 Sep 15;70(2):474-8. doi: 10.1016/j.talanta.2006.02.059. Epub 2006 May 02. PMID: 18970795.
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Talanta. 2006 Sep 15;70(2):474-8. doi: 10.1016/j.talanta.2006.02.059. Epub 2006 May 02.

Pipette tip solid-phase extraction and gas chromatography-mass spectrometry for the determination of mequitazine in human plasma.

Talanta

Takeshi Kumazawa, Chika Hasegawa, Xiao-Pen Lee, Akemi Marumo, Natsuko Shimmen, Akira Ishii, Hiroshi Seno, Keizo Sato

Affiliations

  1. Department of Legal Medicine, Showa University School of Medicine, 1-5-8 Hatanodai, Shinagawa-ku, Tokyo 142-8555, Japan.

PMID: 18970795 DOI: 10.1016/j.talanta.2006.02.059

Abstract

Mequitazine has been found to be extractable from human plasma samples using MonoTip C(18) tips, inside which C(18)-bonded monolithic silica gel was fixed. Human plasma (0.1mL) containing mequitazine and cyproheptadine as an internal standard (IS) was mixed with 0.4mL of distilled water and 25muL of 1M potassium phosphate buffer (pH 8.0). After centrifugation of the mixture, the supernatant fraction was extracted to the C(18) phase of the tip by 25 repeated aspirating/dispensing cycles using a manual micropipettor. The analytes retained on the C(18) phase were then eluted with methanol by five repeated aspirating/dispensing cycles. Without evaporation and reconstitution, the eluate was injected into a gas chromatograph injector and detected by a mass spectrometer with selected ion monitoring in the positive-ion electron impact mode. The separation of mequitazine and the IS from each other and from impurities was generally satisfactory using a DB-1MS capillary column (30mx0.32mm i.d., film thickness 0.25mum). The recoveries of mequitazine and the IS spiked into plasma were more than 90.0%. The regression equation for mequitazine showed excellent linearity in the range of 0.2-200ng0.1mL(-1), and the detection limit was 0.05ng0.1mL(-1)of plasma. The intra-day and inter-day coefficients of variation for mequitazine in human plasma were not greater than 8.16 and 9.24%, respectively. Accuracy for the drug was in the range of 90.0-97.4%. The data obtained from determination of mequitazine in human plasma after oral administration of the drug are also presented.

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