3,4二甲氧基苯乙腈及其杂质的高效液相色谱分析

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武智强， 赵文英*

（青岛科技大学 化工学院，山东 青岛266042）

摘要：建立3,4二甲氧基苯乙腈及其杂质邻苯二酚和藜芦醇的高效液相色谱分析方法。实验采用HPLCDAD，流动相为V(甲醇)∶V(水)=30∶70，BDS C18（46 mm×250 mm，5 μm）色谱柱分离，229 nm波长定量。结果表明，邻苯二酚和藜芦醇的检出限均为1 000 mg·kg-1。3,4二甲氧基苯乙腈、邻苯二酚和藜芦醇标准曲线的r值均大于099。三者高低浓度添加平均回收率990%~1018%，RSD为159%~422%。样品中3,4二甲氧基苯乙腈含量983%，杂质邻苯二酚和藜芦醇含量均低于01%。建立的分析方法高效、实用，能够满足3,4二甲氧基苯乙腈及杂质的定量分析要求。

关键词：3,4二甲氧基苯乙腈； 邻苯二酚； 藜芦醇；HPLCDAD

中图分类号：O 657.7文献标志码：A

Determination of 3,4Dimethoxy Phenyl Acetonitrile and Its Impurities by HPLC

WU Zhiqiang, ZHAO Wenying

(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)

Abstract: A highperformance liquid chromatographic method was developed for analysis of 3,4dimethoxy phenyl acetonitrile and its impuritiespyrocatechol and veratryl alcohol. The method employs a photodiode array detector, a mobile phase consisting of 30% methanol and 70% water, a 4.6 mm× 250 mm BDS C18 column with 5 μm packing, and UV detection at 229 nm. Results show that the LOD of pyrocatechol and veratryl alcohol are 1 000 mg·kg-1. The method demonstrates good linearity in the investigated range with r value all above 0.99. The mean recoveries for high and low fortification level of three standard samples range from 99.0% to 101.8%, and the RSD of the recoveries range between 1.59% and 4.22%. The content of 3,4dimethoxy phenyl acetonitrile in the sample is 98.3%, and pyrocatechol and veratryl alcohol are all under 01%. The method is proven to be efficient and valuable for quantitative analysis of 3,4dimethoxy phenyl acetonitrile and its impurities.

Key words: 3,4dimethoxy phenyl acetonitrile; pyrocatechol; veratryl alcohol; HPLCDAD

 收稿日期：20150122

作者简介： 武智强(1988—)，男，硕士研究生.*通信联系人.

文章编号：16726987（2016）03026505； DOI： 10.16351/j.16726987.2016.03.006