The separation of target compounds and their isomers can be a daunting task particularly when those compounds are present in a highly complex sample matrix. In order to better separate the analytes, several conditions can be tested in the interest of developing a more efficient and effective method. Options for optimization include changing the mobile phase organic modifier and pH, optimizing gradient slope, or adding a second dimension of separation. In this study mobile phase components were varied, and a second separation dimension was added. The resulting 2D-LC method offers better resolution and decreases the chances of target analyte co-elution with matrix components due to the increased peak capacity of the separation. In the study it was found that using methanol and acetonitrile in the first and second dimensions was very important, providing more peak spreading and optimal usage of the 2D separation space. While separations involving acetonitrile in both dimensions were quicker in time, they did not provide the selectivity needed to fully utilize the 2D space. The additional peak capacity of the 2D-LC method was very useful in applying the method to the determination of 14 furanocoumarins in a variety of vegetable matrices. Finally, we compared the precision of quantitation in the 1D and 2D methods and found that while the relative standard deviation of peak area measured at the second dimension detector was slightly worse on average compared to the 1D detector, it was still acceptable, with all %RSDs less than 1.6%.

Optimization of 2D-LC conditions in the separation of furanocoumarins in plant extracts

251st National Meeting (2016)

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