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

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.