Objective: To establish an high performance liquid chromatography (HPLC) coupled with solid phase extraction based on magnetic carbon nanotubes (MCNTs) for the rapid, simple, and efficient determination of norfloxacin in saliva. Methods: First, a new type of magnetic carbon nanotube material based on traditional carbon nanotube material was synthesized as a solid-phase extraction adsorbent. Fourier infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and transmission electron microscopy (TEM) were used to characterize its physical properties. After optimization of extraction conditions, the adsorption performance of MCNTs was applied to enrich norfloxacin in saliva. Then,combined with HPLC, the concentration of norfloxacin was determined by using a C18 column, and a mobile phase of 0.025 mol·L-1 phosphate solution-acetonitrile (87∶13) at a detection wavelength of 278 nm were used. Results: The MCNTs prepared in this study have the characteristics of responsiveness, high adsorption rategreater than 90%, and excellent re-use performance after 12 cycles. In conjunction with HPLC, the content of nofloxacin in saliva was determined at a good linear relationship in the range of 0.4-20 μg·mL-1(r2=0.999 8), which the detection limit was 0.01 ng·mL-1, the quantitative limit was 0.025 ng·mL-1. RSDs of the intra-day and inter-day precision values were both less than 5%, and RSDs of the extraction recovery rate was less than 2%. The concentration of nofloxacin in saliva was 1.902 μg·mL-1. Conclusion: The magnetic solid-phase extraction technology with magnetic carbon nanotubes as adsorbent can be used for the separation, enrichment and detection of norfloxacin in saliva by combining HPLC. The extraction process of this method established is simple, fast, and the content determination is precise and accurate.
FU Lu-lu, CHEN Jin-tao, CHEN Qiu, REN Li-qin, GUO Sheng-nan, JIANG Ya-yang, SHAN Wei-guang
. Determination of norfloxacin in saliva by high performance liquid chromatography combined with magnetic carbon nanotube extraction[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(6)
: 1011
-1018
.
DOI: 10.16155/j.0254-1793.2022.06.13
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