Graphene/multi-walled carbon nanotubes functionalized with an amine-terminated ionic liquid for determination of (Z)-3-(chloromethylene)-6-fluorothiochroman-4-one in urine.
A new type of amine-terminated-ionic-liquid-functionalized graphene/multi-walled carbon nanotubes hybrid material (IL-G/MWCNTs) was synthesized and used as an adsorbent in miniaturized pipette tip solid-phase extraction (PT-SPE) coupled with liquid chromatography for the isolation and determination of (Z)-3-(chloromethylene)-6-fluorothiochroman-4-one (CMFT) in urine. Parameters for the preparation of IL-G/MWCNTs and the PT-SPE procedure, including the mass ratio of graphene oxide and oxidized multi-walled carbon nanotubes, the mass ratio of graphene oxide and the ionic liquid, and the type and volume of washing and elution solvents were optimized to achieve higher extraction efficiency. Good linearity of the method was achieved in the range 0.03-5.0μgmL-1with a coefficient of determination (r2) of 0.9999. The limits of detection and quantification were 0.009 and 0.030μgmL-1, respectively. The intra- and inter-day precisions, expressed as relative standard deviations (RSDs), were evaluated by performing replicate analyses of samples spiked at 0.1μgmL-1on the same day (n=6) and over three consecutive days, and were 4.8 and 5.5%, respectively. Recoveries between 73.9 and 93.9% were obtained at three spiking levels, with RSDs≤7.9%. Five batches of the adsorbent were investigated to confirm the reliability of the preparation method.
Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China.
Huanhuan
H
Chen
Key Laboratory of Analytical Science and Technology of Hebei Province & College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China.
Yanan
Y
Yuan
Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China.
Can
C
Xiang
Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province & College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China. Electronic address: yanhy@hbu.edu.cn.
Hongyuan
H
Yan
Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China.
Yehong
Y
Han
Department of Biochemistry, Baoding University, Baoding 071002, China. Electronic address: qfxbdxy@126.com.
Fengxia
F
Qiao
D000327:Adsorption; D002839:Chromans / Q000652:urine*; D006108:Graphite / Q000737:chemistry*; D052578:Ionic Liquids / Q000737:chemistry*; D008855:Microscopy, Electron, Scanning; D037742:Nanotubes, Carbon / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D012997:Solvents; D017550:Spectroscopy, Fourier Transform Infrared
C000602464:3-(chloromethylene)-6-flourothiochroman-4-one; D002839:Chromans; D052578:Ionic Liquids; D037742:Nanotubes, Carbon; D012997:Solvents; D006108:Graphite
(Z)–3–(chloromethylene)–6–fluorothiochroman–4–one; Amine-terminated-ionic-liquid-functionalized graphene/multi-walled carbon nanotubes; Pipette tip solid-phase extraction; Urine