Molecularly imprinted polymer cartridges coupled to liquid chromatography for simple and selective analysis of penicilloic acid and penilloic acid in milk by matrix solid-phase dispersion

Abstract

A simple, fast and sensitive method for determination of the degradation products of penicillin (penicilloic acid and penilloic acid) in milk samples has been developed by combining selective surface molecularly imprinted matrix solid-phase dispersion and high performance liquid chromatography (SMIPs-MSPD-HPLC). The selected dispersant SMIPs had high affinity for penicilloic acid and penilloic acid in milk matrix and the obtained extract was sufficiently clean for direct injection for HPLC analysis without any interference from the matrix. The proposed SMIPs-MSPD-HPLC method was validated for linearity, precision, accuracy, limit of detection and limit of quantitation. Linearity ranged from 0.04 to 4 μg g(-1) (correlation coefficient r(2) > 0.999). Recoveries of penicilloic acid from milk samples at different spiked levels were between 79.8 and 90.3%, with RSD values within 5.2-7.4%, and the limit of detection and limit of quantitation values were 0.04 and 0.13 μg g(-1), respectively. Recoveries of penilloic acid from milk samples at different spiked levels were between 77.4 and 86.2%, with RSD values within 3.1-6.4%, and the limit of detection and limit of quantitation values were 0.05 and 0.17 μg g(-1), respectively. The developed SMIPs-MSPD-HPLC method was successfully applied to direct determination of penicilloic acid and penilloic acid in milk samples.

Keywords: Degradation products; HPLC; Matrix solid phase dispersion; Surface molecular imprinted polymers.