Dispersive solid-phase microextraction method for sample extraction in the analysis of four tetracyclines in water and milk samples by high-performance liquid chromatography with diode-array detection |
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Authors: | Wen-Hsien Tsai Tzou-Chi Huang Joh-Jong Huang Yi-Huu Hsue Hung-Yi Chuang |
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Institution: | 1. Department of Food Science, National Pingtung University of Science and Technology, Pingtung 912, Taiwan;2. The Health Bureau of Kaohsiung County Government, Kaohsiung County 833, Taiwan;3. School of Public Health, Kaohsiung Medical University, and Department of Community Medicine, Kaohsiung Medical University Hospital, No. 100 Shih-Chuan First Road, Kaohsiung City 807, Taiwan |
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Abstract: | A dispersive solid-phase microextraction (dispersive-SPME) method for the determination of tetracycline, oxytetracycline, chlortetracycline and doxycycline is proposed. Different silica-based and polymeric sorbents were evaluated for their capacity to simultaneously preconcentrate tetracyclines (TCs) in the dispersive format from aqueous or organic solutions. Silica-based sorbents especially functionalized with primary amine, secondary amine, or carbonyl groups have showed higher capacity than polymeric sorbents under organic environment. In the proposed dispersive solid-phase microextraction method, after extraction with acetonitrile and salt-promoted partitioning, TCs were adsorbed to a small amount of dispersive silica-based primary and secondary amine sorbents, desorbed with a small volume of desorption solution, and determined by high-performance liquid chromatography with diode-array detection. Under the optimal conditions, recoveries were determined for surface water and milk samples spiked at 10 ng/mL and 50–150 ng/g, respectively, and quantification was achieved by matrix-matched calibration. The calibration curves of four TCs in both samples showed linearity with a correlation coefficient value above 0.997. Average recoveries ranged from 97.1 to 104.1% and the precision was from 2.0 to 5.6%. Limits of detection ranged from 0.7 to 3.5 ng/mL and from 7.9 to 35.3 ng/g for four TCs surface in surface water and milk samples, respectively. |
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Keywords: | Dispersive solid-phase microextraction Sample preparation Milk analysis Water analysis Tetracyclines |
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