目的 建立HPLC法測(cè)定注射用特利加壓素中有關(guān)物質(zhì)。方法 采用Agilent Poroshell 120EC-C₁₈色譜柱（150 mm×4.6 mm，2.7 μm）；磷酸二氫鉀緩沖液-乙腈（90∶10）為流動(dòng)相A，磷酸二氫鉀緩沖液-乙腈（60∶40）為流動(dòng)相B，梯度洗脫；檢測(cè)波長(zhǎng)為210 nm；體積流量為0.7 mL/min；進(jìn)樣量為20 μL；柱溫為35 ℃。按照主成分對(duì)照品外標(biāo)法計(jì)算。結(jié)果 雜質(zhì)L、K、G、I、D、H、E、F、Y、P、M、B、T、J、N在0.04～40.8 μg/mL線性關(guān)系良好；平均回收率分別為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值分別為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%。結(jié)論 建立的方法準(zhǔn)確、專(zhuān)屬性強(qiáng)，可用于注射用特利加壓素中有關(guān)物質(zhì)的質(zhì)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年國(guó)家藥品抽檢項(xiàng)目(國(guó)藥監(jiān)藥管﹝2023﹞2號(hào))