离子抑制色谱法测定注射用醋酸奥曲肽中乙酸的含量
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篇名: 离子抑制色谱法测定注射用醋酸奥曲肽中乙酸的含量
TITLE:
摘要: 目的:采用离子抑制色谱法测定注射用醋酸奥曲肽中乙酸的含量,为药典标准的完善提供参考。方法:色谱柱为Rezex ROA-Organic Acid H+,流动相为0.002 5 mol/L硫酸溶液,流速为0.5 ml/min,检测波长为210 nm,柱温为45 ℃,进样量为100 μl。结果:乙酸的检测质量浓度线性范围为0.394 4~78.89 μg/ml(r=0.999 9);定量限为197.2 ng/ml,检测限为78.89 ng/ml;精密度、稳定性、重复性试验的RSD<2%;加样回收率为104.71%~109.78%(RSD=1.34%,n=9)。结论:该方法环保、简便、准确度和精密度良好,适用于测定注射用醋酸奥曲肽中乙酸的含量。
ABSTRACT: OBJECTIVE: To determine the content of acetic acid in Octreotide acetate for injection by IEC,and provide reference for the improvement of pharmacopoeia standards. METHODS: The column was Rezex ROA-Organic Acid H+ with mobile phase of 0.002 5 mol/L sulfuric acid at a flow rate of 0.5 ml/min, the detection wavelength was 210 nm, column temperature was 45 ℃, and injection volume was 100 μl. RESULTS: The linear range of acetic acid was 0.394 4 μg/ml-78.89 μg/ml (r=0.999 9); RSDs of precision, stability and reproducibility tests were all lower than 2%; the limit of quantification was 197.2 ng/ml,and limit of detection was 78.89 ng/ml; recovery was 104.71%-109.78%(RSD=1.34%, n=9). CONCLUSIONS: The method is environmental and simple with good accuracy and precision, and suitable for the content determination of acetic acid in Octreotide acetate for injection.
期刊: 2016年第27卷第27期
作者: 李婧华,刘桂霞,李盼盼,王智亮,姚静,李卓荣,山广志
AUTHORS: LI Jinghua,LIU Guixia,LI Panpan,WANG Zhiliang,YAO Jing,LI Zhuorong,SHAN Guangzhi
关键字: 离子抑制色谱法;注射用醋酸奥曲肽;乙酸
KEYWORDS: IEC; Octreotide acetate for injection; Acetic acid
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