柱前衍生HPLC法同时测定阿仑膦酸片中主药及有关物质γ-氨基丁酸的含量  

Simultaneous Determination of Main Components and the Related Substance γ-aminobutyric Acid in Al-endronate Tablets by Pre-column Derivatization HPLC

作　　者：张福成[1] 李海霞[2] 蒋晔[2] 赵静[2] 

机构地区：[1]空军总医院药学部,北京市100036 [2]河北医科大学药学院,石家庄市050017

出　　处：《中国药房》2009年第7期536-538,共3页China Pharmacy

基　　金：河北省自然科学基金资助项目(C2007000792)

摘　　要：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 develop a pre column derivatization HPLC method for the simultaneous determination of the contents of alendronate and the related substance γ aminobutyric acid in alendronate tablets. METHODS： After AccQ pre- column derivatization, the sample was determined with Diamonsil C18 column used as stationary phase and acetonitrile - 35 mmol·L^-1 acetate buffer solution （13.5 ： 86.5, V/V） as a mobile phase. The flow rate was 0.7 mL·min^-1 and the colunto temperature was set at 35 ℃ . RESULTS： Alendronate and γ - aminobutyric acid were well - separated and able to be determined simuhaneously, with their linear ranges at 30.9-990 μg·mL^-1 （r = 0.999 6） and 0.307--960μg·mL^-1 （r = 0.999 9）, respectively and their average recovery rates at 99.3--100.8% and 99.3-100.2%, respectively. The intra- day RSDs of both were no more than 0.8% and their inter- day RSDs were no more than 1.9% . CONCLUSIONS： The method is simple, selective and suitable for the determination of alendronate and the related substance y aminobutyric acid of alendronate tablets.

关 键 词：阿仑膦酸 有关物质 Γ-氨基丁酸 高效液相色谱法 含量测定 

分 类 号：R927.2[医药卫生—药学]