In‐line solid‐phase extraction preconcentration in capillary electrophoresis‐tandem mass spectrometry for the multiresidue detection of quinolones in meat by pressurized liquid extraction

Abstract

We have developed and validated a CE-MS/MS method using an in-line SPE device (analyte concentrator, AC) to determine eight quinolones of veterinary use whose maximum residue levels in animal edible tissues are established by the EU Council Regulation 2377/90, i.e., danofloxacin, sarafloxacin, ciprofloxacin, marbofloxacin, enrofloxacin, difloxacin, oxolinic acid, and flumequine. Different parameters affecting the AC performance, such as its design (in this case frit-free), the kind of sorbent (Oasis MCX), sample pH, volume, and composition of the elution plug and injection time were studied. The method was validated using standard solutions obtaining LODs between 17 and 59 ng/L. Finally, a pressurized liquid extraction (PLE) method was developed to determine these antibiotics in chicken muscle samples. The whole analytical method was validated in terms of linearity (r2 >or= 0.992), recoveries (63-112%), repeatability and intermediate precision (RSD <or= 20%), LODs (40-140 ng/kg) and LOQs (130-470 ng/kg), showing the usefulness of the combination of in-line SPE-CE-MS/MS with PLE for the identification and simultaneous quantification of eight regulated quinolone antibiotics in chicken muscle at very low concentration levels.

Recent food safety and food quality applications of CE‐MS

“…In the last 5 years, and concerning food safety applications, CE-MS has been mostly applied to the determination of different types of pesticides [12][13][14][15][16][17] and antibiotics [18][19][20][21][22][23][24][25][26] in foods and water. Even though, some other interesting applications like the analysis of biogenic amines [27,28], alkaloids [29][30][31], antidepressants [32,33], disinfection byproducts [34], products formed during the processing or cooking of food, such as acrylamides [35], speciation analysis [36][37][38], chemical warfare agent degradation products [39], transgenic foods [30,40] and toxic oligopeptides [41] have also been carried out in this field by CE-MS. Table 1 shows these recent examples of the application of CE-MS.…”

Quick and Sensitive Determination of Fluoroquinolones by Capillary Electrophoresis–Potential Gradient Detection

“…Various detection techniques, e.g., ultraviolet (UV) (Barron et al 2003;JimenezLozano et al 2004;Faria et al 2006), fluorescence (Horstkotter et al 2002;Ferdig et al 2004), mass spectrometry (Juan-Garcia, Font, and Pico 2006;Lara et al 2008), and conductivity detection (CD) (Fan et al 2007) have been combined with CE in the analysis of quinolones. Conductivity detection is based on the conductivity difference between the sample zone and the background electrolyte (BGE).…”

Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection

“…For instance, CE-MS/MS method has been used [7] to determine eight quinolones of veterinary use obtaining limits of detection (LODs) between 17 and 59 ng L −1 . The analytes were extracted from the chicken muscle samples by a pressurized liquid extraction method.…”

“…On the other hand, capillary electrophoresis (CE) and generally highperformance liquid chromatography (HPLC) have been used for the simultaneous determination of quinolones. For instance, some methods that use CE coupled with mass spectrometry have been developed for the quantification of several FQs in milk [6] and chicken [7,8]. Likewise, HPLC with several types of detectors, such as, ultraviolet [9][10][11][12], fluorescence [13][14][15][16] and mass spectrometry [9,11,[17][18][19][20][21] has been employed.…”