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建立了反相离子对色谱法测定兔血清中二氯乙酸钠含量的方法。DCA-Na在碱性条件下加热与水合肼定量生成稳定且有较强吸收系数的腙,以离子对色谱试剂IPR-B_8为对离子,在ZorbaxODS(4.6mm×250mm)柱上,以水-甲醇-IPR-B_8(64:34:2,V/V)为流动相得到较好的分离,灵敏度0.04AUFS,在265nm处测定,衍生物线性范围在0.6~50.0μg/ml,r=0.9994,平均回收率为98.0±3.6%,日内及日间精密度RSD分别为2.6%和3.3%。以本法测定了DCA-Na在兔体内的血药浓度及药代动力学参数。
A method for determination of sodium dichloroacetate in rabbit serum by reversed-phase ion-pair chromatography was established. DCA-Na was heated to hydrazine hydrate quantitatively under alkaline conditions to generate a stable and strong hydrazone with strong absorption coefficient. The ion pair chromatographic reagent IPR-B_8 was used as a counter ion on a Zorbax ODS (4.6 mm × 250 mm) column with water - methanol-IPR-B_8 (64:34: 2, V / V) as the mobile phase, the sensitivity was 0.04AUFS and the peak was at 265nm. The linear range of the derivative was 0.6 ~ 50.0μg / ml , R = 0.9994. The average recovery was 98.0 ± 3.6%. The intra-day and inter-day RSD were 2.6% and 3.3%, respectively. The DCA-Na concentration in plasma and pharmacokinetic parameters were determined by this method.