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  • 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.

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.

Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment (2013-10-22)
S Fan, J H Zou, H Miao, Y F Zhao, H J Chen, R Zhao, Y N Wu
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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ascentis® Express RP-Amide, 2.7 μm Guard Cartridge, 2.7 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 4.6 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm Guard Cartridge, 5 μm particle size, L × I.D. 5 mm × 3 mm, pkg of 3 ea
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® Express RP-Amide, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express RP-Amide, 2 μm UHPLC Column, 2 μm particle size, L × I.D. 7.5 cm × 2.1 mm