Analysis of 27 β-Blockers and Metabolites in Milk Powder by High Performance Liquid Chromatography Coupled to Quadrupole Orbitrap High-Resolution Mass Spectrometry

Abstract

This paper presents an application of high performance liquid chromatography coupled with quadrupole orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the analysis of 27 β-blockers and metabolites in milk powder. Homogenized milk power samples were extracted by acetonitrile and purified by using Oasis PRiME HLB solid-phase extraction cartridges. The Ascentis® C8 chromatographic column was used to separate the analytes. The quantification was achieved by using matrix-matched standard calibration curves with carazolol-d7 and propranolol-d7 as the internal standards. The results show an exceptional linear relationship with the concentrations of analytes over wide concentration ranges (0.5–500 μg kg−1) as all the fitting coefficients of determination r2 are > 0.995. All the limits of detection (LODs) and quantitation (LOQs) values were within the respective range of 0.2–1.5 μg kg−1 and 0.5–5.0 μg kg−1. Overall average recoveries were able to reach 66.1–100.4% with the intra- and inter-day variability under 10%. This method has been successfully applied to the screening of β-blockers and metabolites in commercial milk powders. At the same time, the corresponding characteristic fragmentation behavior of the 27 compounds was explored. The characteristic product ions were determined and applied to the actual samples screening.

Beta-Blocker Separation on Phosphodiester Stationary Phases—The Application of Intelligent Peak Deconvolution Analysis

“…Reliable methods of their analysis are indispensable, especially for determining their purity, for pharmacokinetic and pharmacodynamic studies, metabolism studies (several metabolites are pharmacologically active and harmful), or even for doping control, since some β-blockers are prohibited in athletic competitions [ 1 , 4 , 6 , 7 , 9 ]. Moreover, β-blockers are used to reduce morbidity in animals during their transportation; consequently, these drugs are present in meat or milk [ 11 ]. Appropriate methods of analysis of these compounds are needed for standard substances, drug-active substances, and biological samples (blood, plasma, urine) [ 1 , 4 , 6 , 7 , 9 , 12 , 13 ].…”

“…In most cases, separation has been performed on alkyl stationary phases, such as C18 and C8. The cyano stationary phases and unmodified silica-based columns have also been used [ 4 , 5 , 6 , 9 , 11 , 12 ], as well as monolithic ones [ 7 ]. Mobile phases applied to β-blocker analysis usually consist of different combinations of acetonitrile or methanol with buffers.…”

Rapid and sensitive analysis of trace β-blockers by magnetic solid-phase extraction coupled with Fourier transform ion cyclotron resonance mass spectrometry

“…To date, analytical methods including high-performance liquid chromatography (HPLC) [ 7 , 8 ], two-dimensional HPLC [ 9 ], and HPLC coupled with mass spectrometry (HPLC-MS) [ [10] , [11] , [12] , [13] , [14] , [15] , [16] , [17] ] have been developed for use in the analysis of β-blockers. However, following administration, β-blockers are present at very low concentrations in organisms.…”

“…However, following administration, β-blockers are present at very low concentrations in organisms. In addition, the matrices of biological samples are very complex [ [7] , [8] , [9] , [10] , [11] , [12] , [13] , [14] , [15] , [16] , [17] ], making it cumbersome and time-consuming to analyze these trace-molecules in biological samples. To overcome these limitations, various sample pretreatment methods such as protein precipitation (PP) [ 18 ], matrix solid-phase dispersion [ 19 ], liquid-liquid extraction (LLE) [ 20 ], solid-phase microextraction (SPE) [ 21 , 22 ], and magnetic solid-phase extraction (MSPE) [ 23 , 24 ] have been applied.…”

Determination of β-blocking receptor drugs in silica gel TLC systems with the mobile phase containing surfactant

“…A review on applying high-performance liquid chromatography systems to the analysis of beta-blockers in biological samples was presented in [5]. In [6], the HPLC system linked with Quadrupole Orbitrap High-Resolution Mass Spectrometry was applied to the resolution of 27 betablockers and their metabolites from milk powder samples. In [7], the column-switching (LiChrospher RP-4 and Phenomenex Gemini Phenyl Hexyl 110 A) HPLC-DAD systems were applied, together with gradient of the mobile phase for separation various classes of drug, including beta-blockers Determination of β-blocking receptor drugs in silica gel TLC systems with the mobile phase containing surfactant Current Issues in Pharmacy and Medical Sciences optimise the gradient conditions and successfully applied it to the determination of beta-blockers in the urine sample.…”