HPLC测定硫唑嘌呤片有关物质

HPLC Determination of the Related Substances in Azathioprine Tablets

关键词:  硫唑嘌呤片  有关物质  高效液相色谱法

Key words:  Azathioprine Tablets  related substance  HPLC

摘要:

目的 采用高效液相色谱法测定硫唑嘌呤片有关物质。方法 采用十八烷基硅烷键合硅胶色谱柱(200 mm×4.6 mm，5 μm)，以甲醇-0.05%醋酸钠溶液(18∶82)为流动相，流速为1.2 mL·min^-1，检测波长为300 nm。结果 硫唑嘌呤片中的2个典型杂质6-巯基嘌呤和5-氯-1-甲基-4-硝基咪唑的线性范围均为0.125~1.80 μg·mL^-1(r分别为0.999 7和0.999 9)，检出限分别为0.787 ng和0.933 ng，平均回收率为100.3%(RSD=0.64%)和100.0%(RSD=0.14%)。结论 高效液相色谱法测定硫唑嘌呤片有关物质简便、快速，测定结果准确、可靠。

Abstract:

OBJECTIVE To establish an HPLC method for determination of related substances in Azathioprine Tablets. METHODS The C₁₈ column (200 mm×4.6 mm, 5 μm) was used. The mobile phase consisted of methanol and 0.05% of sodium acetate solution(18∶82) at the flow rate of 1.2 mL·min^-1, and the detection wavelength was set at 300 nm. RESULTS The linear ranges of the two typical related substances mercaptopuring and 5-chloro-1-methyl-4-nitroimidazole in Azathioprine Tablets were all 0.125-1.80 μg·mL^-1(r=0.9997 and 0.9999) with the detection limits of 0.787 ng and 0.933 ng, and the average recoveries were 100.3% and 100.0% with the RSD of 0.64% and 0.14%. CONCLUSION The method proposed for determining the related substances of Azathioprine Tablets is simple, quick and the result is accurate and specific.