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3-    (3-phase HF-LPME)  HPLC-UV/Vis       3(tetracycline, oxytetracycline, chlortetracycline)    .   $C_8$ ( $150{\times}3.0mm$ , $3{\mu}m$ )        .      ,  heptanal,  60,   pH 9.0,   pH 1.0,   700 rpm,   60  5.6~22.3.    $0.08{\sim}0.8{\mu}g/mL$  $0.4{\sim}1.6{\mu}g/mL$ , $0.1{\ sim}32{\mu}g/mL$    ( $R^2$ >0.995) (1.3~9.1 RSD %)  (84~118%) . 【A simple and efficient preconcentration method was developed using three-phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline). The tetracycline antibiotics were separated simultaneously on a column ( $C_8$ , $3.0{\times}150mm$ , $3{\mu}m$ ) with high selectivity and sensitivity using gradient elution. Under optimized conditions (extraction solvent, heptanal; pH of donor, 9.0; pH of acceptor, 1.0; stirring speed, 700 rpm; NaCl salt, 0%; and extraction time, 60 min), enrichment factors (EF) were between 5.6 and 22.3. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of $0.08{\sim}0.8{\mu}g/mL$ and $0.4{\sim}1.6{\mu}g/mL$ , respectively. The calibration curves were linear within the range of $0.1{\sim}32{\mu}g/mL$ with the square of the correlation coefficient being more than 0.995. The precision (as a relative standard deviation, RSD) and accuracy (as a relative recovery) within working range were 1.3~9.1% and 84~118%, respectively.】

Simultaneous Determination of Tetracycline Antibiotics by 3-Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME) and HPLC-UV/Vis