Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 879, Issue 30, Pages 3429-3433Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2011.09.019
Keywords
Ultrasound-assisted IL-DLLME; HPLC; Celastrol; Urine sample
Funding
- National Nature Science Foundation of China [20875095, 21075127, 21105106]
- Nature Science Foundation of Gansu Province [1107RJZA146]
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Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction (UA IL-DLLME) coupled with high-performance liquid chromatography (HPLC) has been developed for the determination of celastrol in human urine samples. In the microextraction procedure, ionic liquid (IL) was used as extraction solvent and dispersed into the aqueous sample solution as fine droplets by means of dispersive solvent and ultrasonication which promoted the analyte to migrate into IL phase more easily. Several important parameters affecting the extraction efficiency were studied and optimized, including the type and volume of extraction solvent and dispersive solvent, sample pH, ultrasonication time, cooling time, centrifugation time and salting-out effect. Under the optimized conditions, 110-fold enrichment factor was obtained and the limit of detection CLOD) was 1.6 mu g/L at a signal-to-noise ratio of 3. The calibration curve was linear over the range of 10-1000 mu g/L for celastrol in human urine sample, with a correlation coefficient of 0.9980. Intra- and inter-assay precision were 0.43% and 2.78%, respectively. The proposed method was successfully applied to the real human urine samples and good spiked recoveries in the range of 93.2-109.3% were obtained. (C) 2011 Elsevier B.V. All rights reserved.
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