HPLC法测定苯丙氨酯原料药及片剂的含量和有关物质

Determination of the related substances and assay of phenprobamate and phenprobamate tablets by HPLC

目的:建立反相高效液相色谱法测定苯丙氨酯及其片剂的有关物质和含量。方法:采用Phenomenex Luna C 18色谱柱(4.6 mm×250 mm,5μm),以甲醇-水(60∶40)为流动相,流速为1.0 mL·min^(-1),检测波长为259 nm,柱温为40℃,进样量为20μL。结果:有关物质线性范围为0.51~30.24μg·mL^(-1),r=0.9999,检出限为4 ng,精密度、稳定性、重复性试验的RSD≤0.8%;含量测定线性范围为12.60~100.82μg·mL^(-1),r=0.9999;苯丙氨酯片的平均回收率为99.7%,RSD=0.6%(n=9);原料含量测定结果为99.3%~99.8%;片剂含量测定结果为99.0%~103.6%。结论:本法简便、准确、专属性好、灵敏度高,可用于苯丙氨酯及其片剂的质量控制。

Objective:To establish an HPLC method for the determination of the related substances and assay of phenprobamate and phenprobamate tablets.Methods:The test was performed on a Phenomenex Luna C 18 column(4.6 mm×250 mm,5μm)with isocratic elution of methanol-water(60∶40).The flow rate was 1.0 mL·min^(-1),and the detection wavelength was set as 259 nm.The column temperature was 40℃,and the injection volume was 20μL.Results:The linear range for the related substances was 0.51-30.24μg·mL^(-1).The limit of detection for the related substances of phenprobamate was 4 ng,and the RSD values of precision,stability and repeatability tests were not more than 0.8%.The linear range for assay of phenprobamate tablets was 12.60^(-1)00.82μg·mL^(-1) with correlation coefficient of 0.9999.The average recovery was 99.7%with a RSD of 0.6%(n=9).The contents of phenprobamate were in the range of 99.3%to 99.8%,and the contents of phenprobamate tablets were in the range of 99.0%^(-1)03.6%.Conclusion:The established method is simple and accurate.It has good specificity and high sensitivity.It can be used for the quality control of phenprobamate and phenprobamate tablets.