Application of the revised EU criteria for the confirmation of anabolic steroids in meat using GC-MS

Abstract

The EU criteria for the confirmation of the presence of illegal compounds in biological matrices were recently revised. The old and the revised criteria were applied to relative ion intensities obtained for five anabolic steroids (methylboldenone, methyltestosterone, ethynylestradiol, beta-boldenone and beta-nortestosterone) in meat (cow, pig, turkey) and fish at concentrations ranging from 0.5 to 5.0 microg/kg. Confirmatory analysis was done by GC-MS; therefore four diagnostic ions had to be monitored and three ion ratios had to be calculated and tested against the criteria. Application of the old and revised criteria, with either standards or fortified samples as reference, showed mutually rather divergent results. Confirmation according to the revised EU criteria and using fortified samples as a reference gave the best results; in other words the highest percentage of diagnostic ion ratios within the tolerance intervals. A correlation was found between the percentage of these ion ratios and the signal/noise (S/N) ratio of the least intense ion of interest in the recorded MS spectrum. Although there were distinct differences in the results obtained for different analytes and sample types, it is safe to conclude that at S/N=3 the percentage of ratios within the tolerance intervals generally will be at or below 50%, while for S/N>/=10, the percentage increases to over 90%. In the present study, fully satisfactory results were obtained down to about 2 microg/kg, but not for lower analyte concentrations.

Confirmation of Pinnatoxins and Spirolides in Shellfish and Passive Samplers from Catalonia (Spain) by Liquid Chromatography Coupled with Triple Quadrupole and High-Resolution Hybrid Tandem Mass Spectrometry

“…Matrix components might influence identification parameters, such as product ion ratio [57], but it was not the case in our study. Product ion ratios were very reproducible in the calibration curves prepared in methanol (<0.5% variation), and the influence of the matrices was completely negligible for PnTX-G ion ratios (<0.3% variation).…”

Determination of anabolic steroids in bovine urine by liquid chromatography–tandem mass spectrometry

“…Also, different techniques have been developed for the determination of anabolic steroids in biological samples. As such high-performance liquid chromatography (HPLC) [3][4][5][6], gas chromatography (GC), GC coupled with mass spectrometry (GC-MS) [7][8][9][10][11][12][13][14][15] GC-high resolution MS [16], GC-MS/MS (mostly on ion traps see [17][18][19][20][21][22][23]) and LC coupled with mass spectrometry (LC-MS) have all been utilized [24][25][26][27][28][29][30][31][32][33][34][35][36].…”

Good quantification practices of flavours and fragrances by mass spectrometry

“…Examples of IPs earned by various MS techniques are given in the electronic supplementary material, table SM-4. Such identification criteria are already implemented in pharmaceutical, veterinary and forensic analyses [30,[32][33][34] and were more recently adopted by the International Organization of the Flavor Industry (IOFI) for the identification of flavouring substances in nature [35]. As a general rule, the positive identification of the target analyte requires that four IPs be obtained, as detailed hereafter for GC-and LC-MS, if the chromatographic resolution is not taken into account (table 2).…”