title: Simultaneous and confirmative detection of multi-residues of β₂-agonists and β-blockers in urine using LC-MS/MS/MS coupled with β-receptor molecular imprinted polymer SPE clean-up.
abstract: A liquid chromatography-linear ion-trap spectrometry (LC-MS³) method using β-receptor molecular-imprinted polymer (MIP) solid-phase extraction (SPE) as clean-up was developed to determine simultaneously and confirmatively residues of 25 β₂-agonists and 21 β-blockers in urine samples. Urine samples were subjected to enzymatic hydrolysis by β-glucoronidase/arylsulphatase, and then extracted with perchloric acid. Sample clean-up was performed using β-receptor MIP SPE. A Supelco Ascentis® express Rp-Amide column was used to separate the analytes, and MS³ detection used an electrospray ionisation source in positive-ion mode. Recovery studies were carried out using blank urine samples fortified with the 46 analytes at the levels of 0.5, 1.0 and 2.0 μg l⁻¹. Recoveries were obtained ranging from 60.1% to 109.9% with relative standard deviations (RSDs, n = 7) from 0.5% to 19.4%. The limits of detection (LODs) and limits of quantitation (LOQs) of the 46 analytes in urine were 0.02-0.18 and 0.05-0.60 μg l⁻¹, respectively. As a result of the selective clean-up by MIP SPE and MS³ detection of the target drugs, the sensitivity and accuracy of the present method was high enough for monitoring β₂-agonist and β-blocker residues in urine samples. Satisfactory results were obtained in the process of the determination of positive urine samples.
authors.affiliation: a Institute of Nutrition and Food Hygiene , Beijing Centre for Disease Control and Prevention , Beijing , China.
authors.forename: S
authors.initials: S
authors.lastname: Fan
authors.forename: J H
authors.initials: JH
authors.lastname: Zou
authors.forename: H
authors.initials: H
authors.lastname: Miao
authors.forename: Y F
authors.initials: YF
authors.lastname: Zhao
authors.forename: H J
authors.initials: HJ
authors.lastname: Chen
authors.forename: R
authors.initials: R
authors.lastname: Zhao
authors.forename: Y N
authors.initials: YN
authors.lastname: Wu
mesh_terms: D000318:Adrenergic beta-Agonists / Q000378:metabolism / Q000652:urine*; D000319:Adrenergic beta-Antagonists / Q000378:metabolism / Q000652:urine*; D053000:Analytic Sample Preparation Methods / Q000662:veterinary; D000818:Animals; D001192:Arylsulfatases / Q000378:metabolism; D002681:China; D002851:Chromatography, High Pressure Liquid / Q000662:veterinary; D005966:Glucuronidase / Q000378:metabolism; D006801:Humans; D006868:Hydrolysis; D055767:Immobilized Proteins / Q000819:agonists / Q000037:antagonists & inhibitors / Q000378:metabolism*; D057230:Limit of Detection; D054802:Molecular Imprinting; D011943:Receptors, Adrenergic, beta / Q000737:chemistry / Q000378:metabolism*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000662:veterinary; D021241:Spectrometry, Mass, Electrospray Ionization / Q000662:veterinary; D015813:Substance Abuse Detection / Q000379:methods / Q000662:veterinary*; D034421:Sus scrofa; D053719:Tandem Mass Spectrometry / Q000662:veterinary
chemical_list: D000318:Adrenergic beta-Agonists; D000319:Adrenergic beta-Antagonists; D055767:Immobilized Proteins; D011943:Receptors, Adrenergic, beta; D001192:Arylsulfatases; D005966:Glucuronidase