右佐匹克隆片中吡嗪-2,3羧酸测定方法的优化

Optimization of determination of pyrazine 2,3-carboxylic acid in dexzopiclone tablets

目的优化高效液相色谱测定右佐匹克隆片中吡嗪-2,3羧酸的方法,解决同一标准对不同厂家右佐匹克隆片中吡嗪-2,3羧酸峰判断和扣除的问题。方法采用高效液相色谱法对多个辅料进行初筛,确定杂质来源后,优化色谱条件,最终采用Venusil MP C18柱(4.6 mm×250 mm,5μm);以水[用磷酸调节pH值至(1.5±0.02)]为流动相A,甲醇为流动相B,梯度洗脱(0~10 min,3%B;10~16 min,3%~80%B;16~25 min,80%B;25.1~35 min,3%B);流速为1.0 mL·min-1;检测波长为270 nm;柱温为30℃;进样量为5μL。结果通过方法学考察,吡嗪-2,3羧酸在0.07975~15.95μg·mL^(-1)内与峰面积线性关系良好,专属性、重复性、稳定性及准确度良好。结论该方法操作简单,结果准确,适用于右佐匹克隆片中吡嗪-2,3羧酸的测定。

Objective To optimize the determination of pyrazine-2,3 carboxylic acid in dexzopicone tablets by HPLC and apply the same standard in judging and deduction of pyrazine-2,3 carboxylic acid peaks in dexzopicone tablets from different manufacturers.Methods HPLC was used to screen multiple materials.After determining the source of impurity,we optimized the chromatography conditions,and ultimately used Venusil MP C18 column(4.6 mm×250 mm,5μm).The mobile phase was water[adjusted to pH(1.5±0.02)with phosphoric acid]as mobile phase A,and methanol as mobile phase B.Gradient elution:0~10 min,3%B;10~16 min,3%~80%B;16~25 min,80%B;and 25.1~35 min,3%B.The flow rate was 1.0 mL·min-1,the detection wavelength was 270 nm,the column temperature was 30℃,and the injection volume was 5μL.Results The linear relationship was good within 0.07975~15.95μg·mL^(-1),with good specificity,repeatability,stability and accuracy.Conclusion The HPLC method can detect pyrazine-2,3 carboxylic acid in dexzopicone tablets with simple operation and accurate results.