PMID- 17536825 OWN - NLM STAT- MEDLINE DCOM- 20070813 LR - 20131121 IS - 0021-8561 (Print) IS - 0021-8561 (Linking) VI - 55 IP - 13 DP - 2007 Jun 27 TI - 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. PG - 4949-56 AB - 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. FAU - Zhang, Yantu AU - Zhang Y AD - College of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China. FAU - Zhang, Zhujun AU - Zhang Z FAU - Sun, Yonghua AU - Sun Y FAU - Wei, Yue AU - Wei Y LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20070531 PL - United States TA - J Agric Food Chem JT - Journal of agricultural and food chemistry JID - 0374755 RN - 0 (Adrenergic beta-Agonists) RN - 10450-60-9 (Periodic Acid) RN - 789U1901C5 (Copper) SB - IM MH - Adrenergic beta-Agonists/*analysis MH - Animals MH - Chromatography, High Pressure Liquid/*methods MH - *Copper MH - Drug Residues/analysis MH - Electrochemistry MH - Food Contamination/*analysis MH - Liver/chemistry MH - Luminescent Measurements MH - Meat/analysis MH - *Periodic Acid MH - Swine EDAT- 2007/06/01 09:00 MHDA- 2007/08/19 09:00 CRDT- 2007/06/01 09:00 PHST- 2007/06/01 09:00 [pubmed] PHST- 2007/08/19 09:00 [medline] PHST- 2007/06/01 09:00 [entrez] AID - 10.1021/jf070144y [doi] PST - ppublish SO - J Agric Food Chem. 2007 Jun 27;55(13):4949-56. doi: 10.1021/jf070144y. Epub 2007 May 31.