离子色谱法同时测定醋酸阿托西班原料药及其注射液中的三氟乙酸与乙酸  

Simultaneous Determination of Trifluoroacetic Acid and Acetic Acid in Atosiban Acetate Bulk Drug and Its Injection by Ion Chromatography

作　　者：严翠霞 张颖 孙珍 陈钢 郑璐侠 邵泓 YAN Cuixia;ZHANG Ying;SUN Zhen;CHEN Gang;ZHENG Luxia;SHAO Hong(NMPA Key Lab.for Quality Control of Therapeutic Monoclonal Antibodies,Shanghai Institute for Food and Drug Control,Shanghai 201203)

机构地区：[1]上海市食品药品检验研究院,国家药品监督管理局治疗类单抗质量控制重点实验室,上海201203

出　　处：《中国医药工业杂志》2023年第1期135-140,共6页Chinese Journal of Pharmaceuticals

基　　金：国家药典委员会课题(2021H058);上海市研发公共服务平台项目(19DZ2294600)。

摘　　要：建立了离子色谱法同时测定醋酸阿托西班(1)原料药及其注射液中的三氟乙酸(2)与乙酸(3)。采用Dionex IonPacTMAS23型阴离子柱(4 mm×25 cm,5μm),以1.0 mmol/L碳酸氢钠溶液和4.0 mmol/L碳酸钠溶液为淋洗液,流速为1.0 mL/min,柱温为30℃,进样量为25μL。结果显示,2、3分别在0.03~11.53μg/mL、0.01~0.20 mg/mL内线性关系良好,定量限分别为1.4、5.1 ng,检测限分别为0.7、2.5 ng。1原料药中2和3的平均加样回收率(n=6)分别为100.9%、101.8%,RSD分别为0.60%、0.74%;1注射液中2和3的平均加样回收率分别为100.4%、101.5%,RSD(n=6)分别为0.86%、0.53%。建立的方法准确、灵敏度高、重复性好,可为1中2的用量控制以及2和3的同时测定提供科学依据。An ion chromatographic method was established for the simultaneous determination of trifluoroacetic acid(2) and acetic acid(3) in atosiban acetate(1) bulk drug and its injection. The Dionex IonPacTMAS23anion column(4 mm×25 cm, 5 μm) was adopted, and the 1.0 mmol/L sodium bicarbonate solution and 4.0 mmol/L sodium carbonate solution were used as eluents. The flow rate was 1.0 mL/min, the column temperature was 30 ℃, and the injection volume was 25 μL. The results showed that it was linear for 2 and 3 in the ranges of 0.03-11.53 μg/mL and 0.01-0.20 mg/mL,respectively. The LOQs of 2 and 3 were 1.4 and 5.1 ng, and the LODs were 0.7 and 2.5 ng, respectively. The average recoveries(n=6) of 2 and 3 in 1 bulk drug were 100.9% and 101.8%, with the RSDs of 0.60% and 0.74%, respectively.The average recoveries(n=6) of 2 and 3 in 1 for injection were 100.4% and 101.5%, with the RSDs of 0.86% and 0.53%,respectively. The established method is accurate, sensitive and reproducible, which can provide a scientific basis for the dosage control of 2 in 1 and the simultaneous determination of 2 and 3 in 1.

关 键 词：离子色谱法 醋酸阿托西班 乙酸 三氟乙酸 

分 类 号：R917[医药卫生—药物分析学]