HPLC法测定多索茶碱注射液中的工艺杂质及降解产物

Determination of process impurities and degradation products in Doxofylline Injection by HPLC

目的 建立多索茶碱注射液有关物质的测定方法。方法采用Agilent TC-C18（4．6 mmx250 mm，5μm）色谱柱；流动相：乙腈一磷酸盐缓冲液（pH 5．0）（20：80）；柱温30℃；流速1．0 mL·min-1；检测波长274 nm。结果茶碱、杂质B、杂质D在0．031～9．62、0．043—9．080、0．126—10．561μg·mL-1浓度范围内，线性关系良好，相关系数r的数值不小于0．999；平均回收率分别为101．4％、99.3％、96．6％，RSD分别为0．3％、0．9％、1．4％（n=9）。结论 建立的方法灵敏度高，测定结果准确，可用于多索茶碱注射液中工艺杂质和降解产物的测定。

Objective To establish an HPLC method for the determination of process impurities and degradation prod-ucts in Doxofylline Injection.Methods The assay was performed on an Agilent TC-C1s column （4.6 mmx250 mm,5 μ）with acetonitrile-phosphate buffer（pH 5.0） （20：80） as mobile phase, the flow rate was 1.0 mL ·min-1, the column tem-perature was 30 ℃ and the detection wavelength was 274 nm.Results Good linearity was obtained in 0.031 -9.62,0.0439.080 and 0.126-10.561 μg · mL-1 for theophylline, impurity B and inmpurity D,respectively.The correlation coefficientwas at least 0.999.The average recovery rates of theophylline, impurity B and impurity D were 101.4% （RSD= 0.3%）,99.3% （ RSD = 0.9% ）, 96.6% （ RSD = 1.4%） , n = 9. Conclusion The method can be used for the determination of processimpurities and degradation products in Doxofylline Injection with high sensitivity, accurate and reliable results.