Confirmation of spectinomycin in milk using ion-pair solid-phase extraction and liquid chromatography-electrospray ion trap mass spectrometry.
A confirmation procedure is described for residues of spectinomycin in bovine milk. Spectinomycin is extracted from raw milk using ion-pair reversed-phase solid-phase extraction. The extracts are ion-pair chromatographed on a polymeric reversed-phase column and analyzed on a quadrupole ion trap mass spectrometer equipped with an electrospray interface. MS-MS data are acquired in the scan mode of product ions deriving from m/z 333, the protonated molecular ion. The estimated limit of confirmation is between 0.05 and 0.1 microg/ml. The procedure was validated with control milk, fortified milk (0.1-5.0 microg/ml), and milk from cows dosed with spectinomycin.
Carson
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MC
Center for Veterinary Medicine, US Food and Drug Administration, Laurel, MD 20708, USA.
Heller
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DN
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D004563:Electrochemistry; D005260:Female; D013058:Mass Spectrometry / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D000198:Spectinomycin / Q000032:analysis*
D000900:Anti-Bacterial Agents; D000198:Spectinomycin