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摘要
建立了高效液相色谱(HPLC)同时测定长春西汀3种中间体杂质残留的分析方法。采用Agilent 5 HC-C18色谱柱,以醋酸铵溶液-乙腈作为流动相,检测波长280 nm,流速1.0 mL/min,柱温35℃,进样量15 μL。结果表明,长春西汀可与阿朴长春胺酸、长春胺酸和长春胺达到完全分离;3种中间体杂质均有良好线性关系(R≥0.999 9),平均回收率均达99.5%以上。本法灵敏、准确、专属性强,可用于长春西汀3种中间体杂质残留的同时测定。
Abstract
A high performance liquid chromatography (HPLC) method for simultaneous determination of three intermediate impurities residues in vinpocetine is established.The chromatographic separation is performed on an Agilent 5 HC-C18 column (5 μm,4.6 mm×250 mm).The mobile phase consists of ammonium acetate solution-acetonitrile (57:43),the flow rate is 1.0 mL/min,the detection wavelength is 280 nm,the column temperature is maintained at 35℃,and the injection volume is 15 μL.It is shown that vinpocetine and the intermediate impurities such as apovincamine acid,vincamine acid and vincamine are separated completely.The calibration curves of three intermediate impurities show good linearity,with average recovery rates all above 99.5%.This method exhibits accurate,sensitive and specific,and can be applied in simultaneous determination of three intermediate impurities residues in vinpocetine.
关键词
高效液相色谱法
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长春胺
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长春胺酸
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阿朴长春胺酸
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中间体杂质
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长春西汀
Key words
high performance liquid chromatography
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vincamine
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vincamine acid
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apovinblastic acid
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intermediate impurities
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vinpocetine
高效液相色谱法同时测定长春西汀3种中间体杂质残留[J].
现代化工, 2020, 40(3): 225-229 DOI:10.16606/j.cnki.issn0253-4320.2020.03.049