高效液相色谱法测定五氯柳胺混悬液的含量及有关物质

为了测定五氯柳胺混悬液的含量和有关物质,建立了一种高效液相色谱法(HPLC)。含量测定方法采用Hypersil BDS C18(150 mm×4.6 mm,5 μm)色谱柱,流动相为0.1%磷酸水-甲醇(体积比为38:62),检测波长为300 nm,柱温为25 ℃。有关物质测定方法采用InertSustainSwift C18(150 mm×4.0 mm,5 μm)色谱柱,流动相、检测波长、柱温与含量测定方法相同。结果表明,五氯柳胺混悬液检测质量浓度线性范围为34.01~104.35 μg·mL^-1(R²=1.000),平均回收率为100.1%;已知杂质2-氨基-4,6-二氯苯酚盐酸盐和3,5,6-三氯水杨酸线性范围为0.51~20.4 μg·mL^-1 (R²分别为0.996、1.000),平均回收率分别为110.3%和98.6%。本研究建立的方法方便、简单、准确,可同时测定五氯柳胺混悬液的含量及有关物质,为该产品的质量控制提供标准。

Determination of related substances and content of oxyclozanide suspension by high performance liquid chromatography

In order to detect the content and related substances of oxyclozanide suspension, a new method using high performance liquid chromatography (HPLC) was established. Content determination was carried out using Hypersil BDS C18 (150 mm×4.6 mm, 5 μm) column and 0.1% phosphoric acid water-method (volume ratio=38:62) as mobile phase, column temperature was 25 ℃, and determination wavelength was 300 nm. Related substances was carried out using InertSustainSwift C18 (150 mm×4.0 mm,5μm) column, mobile phase, detection wavelength and column temperature were the same as the content determination method. The results showed that liner range of content determination of oxyclozanide suspension were 34.01-104.35 μg·mL^-1 (R²=1.000), and average recovery was 100.1%. The liner range of 2-amino-4, 6-dichlorophenol hydrochloride and 3, 5, 6-trichlorosalicylic acid were 0.51-20.4 μg·mL^-1 (R²=0.996, 1.000, respectively), and average recovery were 110.3% and 98.6%, respectively. It showed that the method was convenient, simple and accurate, and could simultaneously determine the content and related substances of oxyclozanide suspension, and provided standards for quality control of the product.