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LIQUID CHROMATOGRAPHY

Determination of Aristocularine Enantiomers by Dispersive Liquid–Liquid Microextraction and Chiral High-performance Liquid Chromatography

, , ORCID Icon & ORCID Icon
Pages 1568-1579 | Received 17 Mar 2016, Accepted 23 Sep 2016, Published online: 31 Jul 2017
 

ABSTRACT

Here is reported a novel analytical approach for the extractive separation and determination of enantiomeric ratios of aristocularine in bovine serum albumin. The results demonstrate suitable analytical performances. The separation was performed by chiral high-performance liquid chromatography with a 5-µm column using a mobile phase of 1:1 n-hexane:ethanol at a flow rate of 0.7 mL min−1 with ultraviolet–visible absorption, circular dichroism, and polarimetric detection. The enantiomers were eluted at 13.2 and 15.6 min for (+) and (−)-aristocularine, with a resolution of 1.58 and a separation factor of 1.27. The analytical parameters for the dispersive liquid–liquid microextraction were optimized; under these conditions, the extraction recoveries were from 88.6% to 93.9% for a two-step extraction. The precision, reported as the percent relative standard deviation, had values from 2.9% to 3.2% for 0.5 µg mL−1 of analyte for five replicate measurements using ultraviolet–visible absorption and circular dichroism detection. The limits of detection were between 0.05 and 0.08 µg mL−1 with enrichment ratios up to a value of 12.

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