UPLC测定注射用醋酸西曲瑞克中有关物质的含量

Determination of Related Substances of Cetrorelix Acetate Injection by UPLC

关键词:  超高效液相色谱法  醋酸西曲瑞克  有关物质

Key words:  UPLC  cetrorelix acetate  related substances

摘要:

b>目的 建立UPLC测定注射用醋酸西曲瑞克的有关物质含量的方法。方法 采用色谱柱ACQUITY UPLC CSHTM C₁₈ (2.1 mm×150 mm，1.7 μm)，流动相A为0.05 mol·L^-1高氯酸钠溶液(磷酸调节pH值至2.0)，流动相B为0.05 mol·L^-1高氯酸钠溶液-乙腈(30∶70)(磷酸调节pH值至2.0)，梯度洗脱，流速为0.2 mL·min^-1，检测波长为226 nm，进样量为1 μL。结果 杂质A、B、C、D、E、F的检测浓度范围分别为0.127 8~6.390 4，0.124 4~6.221 3，0.126 8~6.340 8，0.120 5~6.025 6，0.120 9~6.047 3，0.127 7~6.389 4 μg·mL^-1，各杂质检出限约为0.04 ng，杂质B、D、E定量限约为0.12 ng，杂质A、C、F定量限约为0.13 ng，平均加样回收率分别为97.4%，95.2%，101.5%，105.3%，100.7%，97.4%，RSD分别为1.7%，3.0%，3.8%，2.4%，0.8%，2.8%(n=9)。结论 本方法快速、简便、准确、专属性强，可用于注射用醋酸西曲瑞克中有关物质的定量研究。

Abstract:

OBJECTIVE To establish an UPLC method for determination of related substances of Cetrorelix Acetate injection. METHODS The separation was performed on ACQUITY UPLC CSHTMC₁₈ column(2.1 mm×150 mm, 1.7 μm), 0.05 mol·L^-1 sodium perchlorate solution(adjust the pH with phosphoric acid to 2.0) was used as mobile phase A, and 0.05 mol·L^-1 sodium perchlorate solution-acetonitrile(30︰70)(adjust the pH with phosphoric acid to 2.0) was used as mobile phase B, with a gradient elution. Flow rate was 0.2 mL·min^-1, the detection wavelength was 226 nm and sample volume was 1 μL. RESULTS The linear ranges of impurity A, B, C, D, E and F were 0.127 8-6.390 4, 0.124 4-6.221 3, 0.126 8-6.340 8, 0.120 5-6.025 6, 0.120 9-6.047 3, 0.127 7-6.389 4 μg·mL^-1, respectively. The limits of detection of each impurities was about 0.04 ng. The limits of quantitation of impurity B, D, E were about 0.12 ng, that of impurity A, C, F were about 0.13 ng. The average recoveries were 97.4%, 95.2%, 101.5%, 105.3%, 100.7%, 97.4%, respectively. RSDs were 1.7%, 3.0%, 3.8%, 2.4%, 0.8%, 2.8%(n=9), respectively. CONCLUSION The method is rapid, simple, accurate and specific and can be used for the quantitative study on related substances in Cetrorelix Acetate for injection.