Determination of trace amount of enantiomeric impurity in therapeutic nicotine derivative using capillary electrophoresis with new imaging technology detection

作者：Dahab Ali A^*; Smith Norman W

来源：Journal of Separation Science, 2012, 35(1): 66-72.

DOI：10.1002/jssc.201100513

• Chiral separation
• Enantiomeric impurities
• Highly sulphated beta-cyclodextrin
• Label-free intrinsic imaging

One of the many attempts to stop the danger of tobacco smoking is the development of an anti-smoking vaccine using nicotine butyric acid (NBA) linked to a carrier protein to produce anti-nicotine antibodies. NBA is a chiral molecule and there is a need to obtain a high degree of enantiomeric purity. The aim of this work is to develop a novel method for the enantioseparation of NBA and the determination of trace amounts of enantiomeric impurity required by regulatory authorities. This was achieved successfully using high-performance capillary electrophoresis combined with label-free intrinsic imaging as new imaging technology. A 50 mu m id fused-silica capillary was used with UV detection at lambda(214) nm and label-free intrinsic imaging. The background electrolyte consisted of highly sulphated beta-cyclodextrin 10% m/V as a chiral selector in 75 mM phosphoric acid-triethylamine at pH 7.0. Baseline separation and detection of 0.1% and possibly less of the unwanted impurity (R-enantiomer) were achieved. Also, the detection limits were calculated for both enantiomers. The use of label-free intrinsic imaging has improved the sensitivity, enabling us to detect trace amounts of enantiomeric impurities.

• 出版日期2012-1