篇名: HPLC法测定硫辛酸注射液中的有关物质
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pH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20 μl。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0.828~52.992 μg/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。
ABSTRACT: 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 pH 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.
期刊: 2016年第27卷第21期
作者: 夏天水,熊全红,罗云龙
AUTHORS: XIA Tianshui,XIONG Quanhong,LUO Yunlong
关键字: 硫辛酸注射液;高效液相色谱法;有关物质
KEYWORDS: Thioctic acid injection; HPLC; Related substances
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