Multiclass Residues Screening of 105 Veterinary Drugs in Meat, Milk, and Egg Using Ultra High Performance Liquid Chromatography Tandem Quadrupole Time-of-Flight Mass Spectrometry

Abstract

& A high-throughput and robust method for analyzing multiclass residues of veterinary drugs in meat, milk, and egg by ultra-high performance liquid chromatography (UHPLC)-quadrupole time-of-flight mass spectrometry (QTOF) was established. The method successfully applied to the screening, quantification, and confirmation of 105 compounds from 9 different classes of drugs, including beta-agonists, benzimidazoles, corticoides, triphenylmethane, nitromidazoles, quinolones, sulfonamides, tetracylines, and benzodiazepams. The samples are extracted by a single extraction using acetonitrile containing 0.1% formic acid, followed by an easy solid phase extraction (SPE) clean-up on HLB column and finally analyzed by LC=MS QTOF MS. The separation was achieved within 30 min at the optimized chromatographic conditions. More than 92% compounds in this study can be reliably identified based on accurate mass measurement (within the 3 ppm mass error) at the 5 lg=kg concentration levels in the complex food matrix with further MS=MS confirmation. Our study demonstrated a reliable, high-efficient and high-sensitive strategy for the fast and high throughput screening of multiclass of veterinary drugs in foodstuffs of animal origin.

Multiclass and multiresidue screening of veterinary drugs and pesticides in infant formula using Quadrupole‐Orbitrap MS with PRM scan mode

“…As a medium polar solvent and protein precipitant, acetonitrile is commonly applied to multiresidue extraction. It was reported that acidic acetonitrile could improve extraction of quite a lot of compounds and FA was the most frequently used modifier . In this study, 0.5% FA in acetonitrile achieved higher recoveries for most analytes.…”

Multiresidue method for the determination of pharmacologically active substances in egg and honey using a continuous solid-phase extraction system and gas chromatography–mass spectrometry

“…The end result is poor isolation and purification of PASs, which can be avoided by removing lipids and proteins before analysis (Shim, Lee, Kim, Lee, & Kim, 2003). Acetonitrile is the preferred extraction solvent for this purpose by virtue of its excellent hydrophilic and lipophilic extraction performance in combination with various modifiers such as water (Peters et al, 2009), formic acid (Deng et al, 2011) or phosphate (Herranz, Moreno-Bondi, & Marazuela, 2007). Ethyl acetate-acetonitrile-ammonium hydroxide mixtures have also been used to extract various antibiotics from egg samples (Xie et al, 2011).…”

“…However, the low volatility of some PAS and the presence of various polar groups in others require the use of an appropriate derivatization procedure to obtain more volatile products. In recent years, several methods based on liquid chromatography-mass spectrometry (Huang et al, 2006), tandem mass spectrometry (Ashwin et al, 2005;Bohm et al, 2012;Garrido Frenich et al, 2010;Martinez Vidal et al, 2009;Wang et al, 2014), mass time-of-flight mass spectrometry (Peters, Bolck, Rutgers, Stolker, & Nielen, 2009) and tandem quadrupole time-of-flight mass spectrometry detection (Deng et al, 2011) have been successfully used to determine PASs in eggs, honey and other food commodities with good sensitivity and selectivity. Recently, methodologies using ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry have been developed for the separation and detection of pesticides and veterinary drugs in honey (Gómez-Pérez et al, 2012) or baby food (Jia, Chu, Ling, Huang, & Chang, 2014).…”

“…In most cases, analytes are extracted from theses matrices by liquid-liquid extraction, occasionally with the aid of solid-phase extraction (SPE) for cleanup purposes (Hao, Zhao, & Yang, 2007). The hydrophilic-lipophilic balanced sorbent Oasis HLB is the most widely used for extracting polar and nonpolar pharmaceutical compounds (Bohm, Stachel, & Gowik, 2012;Deng et al, 2011;Garrido Frenich, del Mar Aguilera-Luiz, Martínez Vidal, & Romero-González, 2010;Martinez Vidal et al, 2009;Sánchez-Brunete, Albero, Miguel, & Tadeo, 2005). Other sorbents such as silica (Courant et al, 2007(Courant et al, , 2008, Strata-X (Ashwin, Stead, Taylor, Startin, & Richmond, 2005), RP-C18 (Rejtharová & Rejthar, 2009) and molecularly imprinted polymers (Blasco & Picó, 2012;Rejtharová & Rejthar, 2009) have also been used for the SPE of PASs from eggs and honey.…”

The Assessment of Selectivity in Different Quadrupole-Orbitrap Mass Spectrometry Acquisition Modes

“…Currently, HR-MS is used in screening [17][18][19][20] as well as confirmatory analysis of drug residues [21,22]. HR-MS is specifically mentioned in 2002/657/EC [1] but neither unequivocal criteria for the minimum resolution needed nor for allowed mass deviations are specified.…”