目的 建立HPLC法测定注射用特利加压素中有关物质。方法 采用Agilent Poroshell 120EC-C₁₈色谱柱（150 mm×4.6 mm，2.7 μm）；磷酸二氢钾缓冲液-乙腈（90∶10）为流动相A，磷酸二氢钾缓冲液-乙腈（60∶40）为流动相B，梯度洗脱；检测波长为210 nm；体积流量为0.7 mL/min；进样量为20 μL；柱温为35 ℃。按照主成分对照品外标法计算。结果 杂质L、K、G、I、D、H、E、F、Y、P、M、B、T、J、N在0.04～40.8 μg/mL线性关系良好；平均回收率分别为99.46%、98.35%、98.24%、99.15%、100.01%、99.34%、99.56%、99.42%、98.79%、98.64%、99.16%、98.22%、99.31%、98.11%、99.38%，RSD值分别为0.98%、1.23%、1.45%、0.85%、1.21%、1.09%、1.16%、0.94%、1.25%、0.79%、1.42%、0.92%、0.88%、1.72%、1.26%。结论 建立的方法准确、专属性强，可用于注射用特利加压素中有关物质的质量控制。

Objective To establish an HPLC method for determination of substances in Terlipressin for injection. Methods Agilent Poroshell 120EC-C₁₈ column (150 mm×4.6 mm, 2.7 μm) was used. Mobile phase A was potassium dihydrogen phosphate buffer - acetonitrile (90:10), mobile phase B was potassium dihydrogen phosphate buffer - acetonitrile (60:40), and gradient elution was carried on. Detection wavelength was set at 210 nm, volume flow rate was 0.7 mL/min, and injection volume was 20 μL. Column temperature was 35 ℃. The related substances were calculated using the principal component reference standard external standard method. Results The linear range of impurities L, K, G, I, D, H, E, F, Y, P, M, B, T, J, and N was 0.04 — 40.80 μg/mL. The average recovery was 99.46%, 98.35%, 98.24%, 99.15%, 100.01%, 99.34%, 99.56%, 99.42%, 98.79%, 98.64%, 99.16%, 98.22%, 99.31%, 98.11%, and 99.38%, respectively, and the RSD value was 0.98%, 1.23%, 1.45%, 0.85%, 1.21%, 1.09%, 1.16%, 0.94%, 1.25%, 0.79%, 1.42%, 0.92%, 0.88%, 1.72%, and 1.26%. Conclusion The established method is accurate and highly specific, and can be used for quality control of related substances in Terlipressin for injection.

R917

2023年国家药品抽检项目(国药监药管﹝2023﹞2号)