GC测定丙戊酸钠缓释片的有关物质

Determination of Related Substances in Compound Sodium Valproate and Valproic Acid SR Tablets by GC

关键词:  丙戊酸钠缓释片  有关物质检测  气相色谱法

Key words:  Compound Sodium Valproate and Valproic Acid SR tablets  detection of related substances  GC

摘要:

目的 建立毛细管气相色谱法检测丙戊酸钠缓释片有关物质的方法。方法 采用聚乙二醇为固定液的HP-FFAP色谱柱（30 m×0.53 mm，1 μm），柱温为程序升温；氮气为载气，流速为10 mL·min^-1；直接进样1.0 μL，进样口温度200℃；采用氢火焰离子化检测器，检测器温度250℃。结果 建立的方法专属性强，能有效分离丙戊酸钠缓释片中的10个杂质；丙戊酸在1.01~8.06 μg·mL^-1内线性关系良好（r=0.998 2，n=5），最低检出限为0.403 μg·mL^-1。方法重复性良好，各杂质加样回收率均>90%，且RSD均<5%。结论 该方法可用于丙戊酸钠缓释片的有关物质检测。

Abstract:

OBJECTIVE To develop a capillary gas chromatography(GC) method for determination of related substances in Compound Sodium Valproate and Valproic Acid SR tablets. METHODS The CGC column was PEG-20M(HP-FFAP, 30 m×0.53 mm, 1 μm), temperature programming. N₂ as carrier gas (flow rate:10 mL·min^-1). The temperature of the injection port was maintained at 200℃, and that of the flame-ionization detector(FID) was 250℃. The injection volume was 1.0 μL. RESULTS The method was specific. Valproic acid had a good linear relationship in the range of 1.01-8.06 μg·mL^-1(r=0.998 2, n=5) and the lowest limit of detection was 0.403 μg·mL^-1. The relative recovery was >90%, and the RSD was <5%. CONCLUSION The method can be used for the determination of related substances in Compound Sodium Valproate and Valproic Acid SR tablets.