Two rapid, sensitive and reproducible methods for the determination of baclofen( BAL) in urine and plasma based on high-performance liquid chromatography (HPLC) with UV-vis and fluorescent detection, respectively, were developed for the first time using a new synthesized fluorescent label, 6-oxy-(N-succinimidylacetate)-9-(2′-methoxycarbonyl) fluorescein (SAMF). The optimal derivatization yield was achieved in borate buffer (pH 8.0) for 15 min at room temperature (25 °C). With a mixture of methanol and water containing 5 mmol L-1 sodium citrate buffer (pH 5.0) as mobile phase, BAL was determined at λ = 455 nm with UV-vis detection and at λex/λem = 488/520 nm with FD detection. The detection limits are 1.065 × 10-3 mg mL-1 and 1.065 × 10-2 mg mL-1 with HPLC-UV-vis and HPLC-FD, respectively. The proposed method has been successfully applied to the analysis of BAL in human urine and plasma samples. The established method is rapid (15 min of derivatization process and 10 min of chromatographic run), reproducible and sensitive.
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