Kelly J W, Stewart J T, Blanton C D
Department of Medicinal Chemistry, College of Pharmacy, University of Georgia, Athens 30602-2352.
Biomed Chromatogr. 1994 Sep-Oct;8(5):255-7. doi: 10.1002/bmc.1130080512.
A stereospecific HPLC method was developed for the analysis of (-) and (+) pentazocine in human serum. Each enantiomer and the internal standard nalophine were isolated from serum using a liquid-liquid extraction procedure. Recoveries of 99.05 +/- 5.37 and 97.42 +/- 2.78% were obtained for (-) and (+) pentazocine, respectively. Resolution of the enantiomers was obtained by using an ovomucoid chiral stationary phase with a mobile phase of methanol:acetonitrile: 10 mM phosphate buffer, pH 5.8 (20:5.3:74.7 v/v/v). A resolution (Rs) value of 1.80 was obtained for the pentazocine enantiomers. Linear calibration curves were obtained in the 10-100 ng/mL range for each enantiomer in serum. The detection limit based on a signal-to-noise ratio of 3 was 5 ng/mL for each enantiomer in serum using fluorescence detection with excitation at 275 nm and emission set at 335 nm. The lowest quantifiable level was found to be 10 ng for each enantiomer. Precision and accuracy of the method were in the 3.8-4.8% and 1.3-4.2% ranges, respectively.
建立了一种立体专一性高效液相色谱法，用于分析人血清中的（-）和（+）喷他佐辛。采用液-液萃取法从血清中分离出每种对映体和内标纳络芬。（-）和（+）喷他佐辛的回收率分别为99.05±5.37%和97.42±2.78%。使用卵类粘蛋白手性固定相，流动相为甲醇：乙腈：10 mM磷酸盐缓冲液，pH 5.8（20:5.3:74.7 v/v/v），实现了对映体的分离。喷他佐辛对映体的分离度（Rs）值为1.80。血清中每种对映体在10-100 ng/mL范围内获得了线性校准曲线。使用荧光检测，激发波长为275 nm，发射波长为335 nm，血清中每种对映体基于3:1信噪比的检测限为5 ng/mL。每种对映体的最低可定量水平为10 ng。该方法的精密度和准确度分别在3.8-4.8%和1.3-4.2%范围内。
