Deng Dongli, Deng Hao, Zhang Lichun, Su Yingying
1Engineering Research Center of Chemical Zero Discharge & Department of Chemical Engineering, Chongqing Industry Polytechnic College, Chongqing 401120, China.
J Chromatogr Sci. 2014 Apr;52(4):357-62. doi: 10.1093/chromsci/bmt039. Epub 2013 Apr 25.
A simple and rapid capillary electrophoresis method was developed for the separation and determination of ephedrine (E) and pseudoephedrine (PE) in a buffer solution containing 80 mM of NaH2PO4 (pH 3.0), 15 mM of β-cyclodextrin and 0.3% of hydroxypropyl methylcellulose. The field-amplified sample injection (FASI) technique was applied to the online concentration of the alkaloids. With FASI in the presence of a low conductivity solvent plug (water), an approximately 1,000-fold improvement in sensitivity was achieved without any loss of separation efficiency when compared to conventional sample injection. Under these optimized conditions, a baseline separation of the two analytes was achieved within 16 min and the detection limits for E and PE were 0.7 and 0.6 µg/L, respectively. Without expensive instruments or labeling of the compounds, the limits of detection for E and PE obtained by the proposed method are comparable with (or even lower than) those obtained by capillary electrophoresis laser-induced fluorescence, liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. The method was validated in terms of precision, linearity and accuracy, and successfully applied for the determination of the two alkaloids in Ephedra herbs.
开发了一种简单快速的毛细管电泳方法,用于在含有80 mM磷酸二氢钠(pH 3.0)、15 mM β-环糊精和0.3%羟丙基甲基纤维素的缓冲溶液中分离和测定麻黄碱(E)和伪麻黄碱(PE)。采用场放大进样(FASI)技术对生物碱进行在线富集。与传统进样相比,在存在低电导率溶剂塞(水)的情况下使用FASI,灵敏度提高了约1000倍,且分离效率没有任何损失。在这些优化条件下,两种分析物在16分钟内实现了基线分离,E和PE的检测限分别为0.7和0.6 μg/L。该方法无需昂贵仪器或对化合物进行标记,所获得的E和PE的检测限与毛细管电泳激光诱导荧光、液相色谱-串联质谱和气相色谱-质谱法相当(甚至更低)。该方法在精密度、线性和准确性方面得到了验证,并成功应用于麻黄草中两种生物碱的测定。