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Open AccessArticle

Automated Analysis of Oxytocin by On-Line in-Tube Solid-Phase Microextraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry

School of Pharmacy, Shujitsu University, 1-6-1, Nishigawara, Okayama 703-8516, Japan
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Academic Editor: Mary Boyce
Chromatography 2015, 2(3), 382-391; https://doi.org/10.3390/chromatography2030382
Received: 12 May 2015 / Revised: 21 June 2015 / Accepted: 26 June 2015 / Published: 30 June 2015
(This article belongs to the Special Issue Solid Phase Micro-Extraction)
A simple and sensitive method for the analysis of oxytocin was developed using automated on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC–MS/MS). Oxytocin was separated within 3 min on a Zorbax Eclipse XDB-C8 column, with water/methanol (10/90, v/v) as the mobile phase at a flow rate of 0.2 mL min−1. Electrospray ionization conditions in the positive ion mode were optimized for MS/MS detection by multiple reaction monitoring. The optimum in-tube SPME conditions were 20 draw/eject cycles of 40 µL sample at a flow rate of 250 µL min−1 using a Supel-Q PLOT capillary column as an extraction device. The extracted oxytocin was easily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. The calibration curves for oxytocin were linear (r = 0.9981) in the range of 0−5.0 ng mL−1, and the relative standard deviations at each point were below 14.7% (n = 3). The limit of detection of this method was 4.0 pg mL−1, and its sensitivity was 58-fold higher than that of the direct injection method. This method was applied successfully to the analysis of oxytocin in saliva samples without any other interference peaks. View Full-Text
Keywords: in-tube solid-phase microextraction; oxytocin; saliva; liquid chromatography-tandem mass spectrometry in-tube solid-phase microextraction; oxytocin; saliva; liquid chromatography-tandem mass spectrometry
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Moriyama, E.; Kataoka, H. Automated Analysis of Oxytocin by On-Line in-Tube Solid-Phase Microextraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry. Chromatography 2015, 2, 382-391.

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