中国药房2012，Vol.23Issue(25)：2372-2373,2.DOI:10.6039/j.issn.1001-0408.2012.25.26
柱前衍生化顶空气相色谱法同时检测非布司他原料药中3种微量有机酸
Simultaneous Determination of 3 Kinds of Trace Organic Acids in Febuxostat by Headspace GC with Pre-column Derivatization
朱圣亮 1李语如 1宋晓光1
作者信息
- 1. 江苏恒瑞医药股份有限公司研究院,江苏连云港222047
- 折叠
摘要
Abstract
OBJECTIVE: To establish a method for the content determination of 3 kinds of trace organic acids in febuxostat, such as trifluoroacetic acid, formic acid and acetic acid. METHODS: GC method was adopted. The pre-column derivatization of organic acids was conducted with the mixture of methanol and H2SO4. Then the content of organic acid in 5 batches of samples were determined by headspace GC. The separation was performed on Supelpowax-10 capillary column with FID as the detector. The injection temperature was 160 X,, the detector temperature was 260 ℃, with temperature programming. N2 was used as carrier gas and split ratio was 10:1. Vial equilibration temperature was 60 ℃ with equilibration time of 60 min. RESULTS: The baseline resolution was achieved between the derivatives of three organic acids. The linear ranges were 4.190~605.3μg·mL-1, 3.586～672.5 μg· mL-1, 3.773～667.4 μg·mL-1 (r≥0.999 0). The detective limits were 1.25, 1.07 and 1.13 μg·mL-1 respectively. No organic acid was found in 5 batches of samples. CONCLUSION: The method is accurate and rapid, and can be used for effective separation and content determination of 3 trace organic acids in febuxostat.关键词
项空气相色谱法/柱前衍生化/非布司他/有机酸/测定Key words
Headspace GC/ Pre-column derivatization/ Febuxostat/ Organic acids/ Determination分类
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朱圣亮,李语如,宋晓光..柱前衍生化顶空气相色谱法同时检测非布司他原料药中3种微量有机酸[J].中国药房,2012,23(25):2372-2373,2.
