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目的:建立以柱前衍生高效液相色谱法同时测定阿仑膦酸片中主药及有关物质γ-氨基丁酸含量的方法。方法:样品经AccQ柱前衍生后,以Diamonsil C18为固定相,乙腈-35mmol·L-1醋酸盐缓冲溶液(13.5∶86.5,V/V)为流动相,流速为0.7mL·min-1,柱温为35℃。结果:主药阿仑膦酸及有关物质γ-氨基丁酸分离良好且能够被同时检测;二者检测浓度线性范围分别为30.9～990(r=0.999 6)、0.307～960μg·mL-1(r=0.999 9),回收率分别为99.3%～100.8%、99.3%～100.2%,日内RSD均≤0.8%,日间RSD均≤1.9%。结论:本方法操作简单、选择性好,可用于阿仑膦酸及其有关物质γ-氨基丁酸的含量测定。
OBJECTIVE: To establish a method for the simultaneous determination of γ-aminobutyric acid and its metabolites in alendronate tablets by high performance liquid chromatography (HPLC). Methods: The sample was pre-column derivatized with AccQ, with Diamonsil C18 as stationary phase and acetonitrile-35 mmol·L-1 acetate buffer solution (13.5: 86.5, V / V) as mobile phase at a flow rate of 0.7 mL · min -1 The column temperature was 35 ° C. Results: The main drug alendronate and its related substances γ-aminobutyric acid were well separated and could be detected simultaneously. The linear range of the two drugs were 30.9-990 (r = 0.999 6), 0.307-960μg · mL -1 r = 0.999 9). The recoveries were 99.3% -100.8% and 99.3% -100.2%, respectively. The intraday RSDs were all ≤0.8%, and the daytime RSDs were both ≤1.9%. Conclusion: The method is simple, selective and can be used for the determination of γ-aminobutyric acid of alendronate and its related substances.