title: Development of an analytical method for the determination of beta2-agonist residues in animal tissues by high-performance liquid chromatography with on-line electrogenerated [Cu(HIO6)2]5- -luminol chemiluminescence detection.
abstract: A novel method was developed for the simultaneous determination of beta2-agonist residues such as terbutaline, salbutamol, and clenbuterol by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection. The procedure was based on the enhancement effect of beta2-agonists on the CL reaction between luminol and the complex of trivalent copper and periodate ([Cu(HIO6)2]5-), which was on-line electrogenerated by constant current electrolysis. The HPLC separation used a Nucleosil RP-C18 column (250 mm x 4.6 mm i.d., 5 microm; pore size, 100 A) with a mobile phase consisting of 90% acetonitrile and 10% aqueous ammonium acetate (20 mmol L-1, pH 4.0) at a flow rate of 1.0 mL min-1. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Liver samples were hydrolyzed with beta-glucuronidase followed by a solid-phase extraction procedure using Waters OasisMCX cartridges. Under optimum conditions, the limits of detection at a signal-to-noise ratio of 3 ranged from 0.007 to 0.01 ng g-1 and the limits of quantification at a signal-to-noise ratio of 10 ranged from 0.023 to 0.033 ng g-1 for three beta2-agonists. The relative standard deviations (RSDs) of intra- and interday precision were below 4.5%. The average recoveries for beta2-agonists (spiked at the levels of 0.05-5.0 ng g-1) in pig liver ranged from 84 to 110%, and the RSDs of the quantitative results were from 1.6 to 7.2%. The proposed method was successfully applied to the determination of beta2-agonist residues in pig liver samples.
authors.affiliation: College of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China.
authors.forename: Yantu
authors.initials: Y
authors.lastname: Zhang
authors.forename: Zhujun
authors.initials: Z
authors.lastname: Zhang
authors.forename: Yonghua
authors.initials: Y
authors.lastname: Sun
authors.forename: Yue
authors.initials: Y
authors.lastname: Wei
mesh_terms: D000318:Adrenergic beta-Agonists / Q000032:analysis*; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003300:Copper; D004350:Drug Residues / Q000032:analysis; D004563:Electrochemistry; D005506:Food Contamination / Q000032:analysis*; D008099:Liver / Q000737:chemistry; D008163:Luminescent Measurements; D008460:Meat / Q000032:analysis; D010504:Periodic Acid; D013552:Swine
chemical_list: D000318:Adrenergic beta-Agonists; D010504:Periodic Acid; D003300:Copper