摘要
目的:建立测定硫辛酸注射液中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Agilent Eclipse Plus C18,流动相A为0.005 mol/L磷酸二氢钾溶液(用磷酸调节p H至3.0~3.1)、流动相B为甲醇-乙腈(1∶1,V/V)(梯度洗脱),流速为1.2 ml/min,检测波长为215 nm,柱温为35℃,进样量为20μl。结果:在所建立的色谱条件下,硫辛酸与各杂质及其降解产物分离良好;硫辛酸检测质量浓度线性范围为0.828~52.992μg/ml(r=0.999 9);精密度、稳定性试验的RSD〈3%;杂质A的加样回收率为98.45%~105.73%,RSD=2.41%(n=9);其最大未知单个杂质的质量分数为0.152%~0.189%,总杂质的质量分数为0.487%~0.516%。结论:该方法简便、准确、专属性强、灵敏度高,可用于硫辛酸注射液中有关物质的测定。
OBJECTIVE:To establish a method for the determination of related substances in Thioctic acid injection. METHODS:HPLC was performed on the column of Agilent Eclipse Plus C18 with mobile phase A of 0.005 mol/L potassium dehydrogenate phosphate solution(adjusted with phosphoric acid to p H 3.0 to 3.1)and B of methanol:aoetonitrile(1∶1,V/V)(gradient elution)at a flow rate of 1.2 ml/min;detection wavelength was 215 nm,column temperature was 35 ℃,and the injection volume was 20 μl. RESULTS:Under the established chromatographic conditions,thioctic acid with impurities and its degradation products were well separated;the linear range of thioctic acid was 0.828-52.992 μg/ml(r=0.999 9);RSDs of precision and stability tests were lower than 3%;recovery of impurity A was 98.45%-105.73%(RSD=2.41%,n=9);the largest single impurity content in mass fraction was 0.152%-0.189%,the total impurity content in mass fraction was 0.487%-0.516%. CONCLUSIONS:The method is simple,accurate,specific and sensitivity,and can be used to determine the related substances of the Thioctic acid injection.
出处
《中国药房》
CAS
北大核心
2016年第21期2980-2982,共3页
China Pharmacy