改进HPLC法测定吲哚美辛肠溶片中的有关物质
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篇名: 改进HPLC法测定吲哚美辛肠溶片中的有关物质
TITLE:
摘要: 目的:改进高效液相色谱法测定吲哚美辛肠溶片中2-甲基-5-甲氧基-1H-吲哚-3-乙酸(以下简称杂质Ⅰ)和4-氯苯甲酸(以下简称杂质Ⅱ)的含量。方法:色谱柱为Phenomenex Phenyl-Hexyl,流动相为10 g/L醋酸溶液-乙腈(梯度洗脱),流速为1.0 ml/min,检测波长为254 nm,柱温为40 ℃,进样量为20 μl。结果:杂质Ⅰ和杂质Ⅱ的检测质量浓度线性范围分别为0.262 2~5.243 0、0.252 5~5.050 0 μg/ml(r均为0.999 8);定量限分别为1.12、0.48 ng,检测限分别为0.340、0.146 ng;精密度、稳定性、重复性试验的RSD<2%;杂质Ⅰ和杂质Ⅱ的加样回收率分别为99.71%~100.52%(RSD=0.28%,n=9)、100.84%~102.14%(RSD=0.47%,n=9)。结论:该方法准确、快速,可用于吲哚美辛肠溶片中杂质Ⅰ和杂质Ⅱ的含量测定。
ABSTRACT: OBJECTIVE: To improve HPLC for the contents determination of 2-methyl-5-methoxy-indole-3-acetic acid (impurity Ⅰ) and 4-chlorobenzoic (impurity Ⅱ) in Indometacin enteric-coated tablet. METHODS: The column was Phenomenex Phenyl-Hexyl with mobile phase of 10 g/L acetic acid solution - acetonitrile (gradient elution) at a flow rate of 1.0 ml/min, the detection wavelength was 254 nm, column temperature was 40℃, injection volume was 20 μl. RESULTS: The linear range was 0.262 2-5.243 0 μg/ml for impurity Ⅰ (r=0.999 8) and 0.252 5-5.050 0 μg/ml for impurity Ⅱ (r=0.999 8); the limits of quantitation were 1.12 ng and 0.48 ng, limits of detection were 0.340 ng and 0.146 ng, respectively; RSDs of precision, stability and reproducibility tests were lower than 2%; recoveries were 99.71%-100.52% (RSD=0.28%,n=9) and 100.84%-102.14%(RSD=0.47%,n=9). CONCLUSIONS: The method is accurate and rapid, and can be used for the contents determination of impurity Ⅰ and impurity Ⅱ in Indometacin enteric-coated tablet.
期刊: 2016年第27卷第27期
作者: 李超
AUTHORS: LI Chao
关键字: 高效液相色谱法;吲哚美辛肠溶片;2-甲基-5-甲氧基-1H-吲哚-3-乙酸;4-氯苯甲酸
KEYWORDS: HPLC; Indometacin enteric-coated tablet; 2-methyl-5-methoxy-indole-3-acetic acid; 4-chlorobenzoic
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