Confirmation of sulfamethazine, sulfathiazole, and sulfadimethoxine residues in condensed milk and soft-cheese products by liquid chromatography/tandem mass spectrometry.
A liquid chromatography/tandem mass spectrometry method (LC/MS/MS) is described for the simultaneous detection of 3 sulfonamide drug residues at 1.25 ppb in condensed milk and soft-cheese products. The 3 sulfonamide drugs of interest are sulfathiazole (STZ), sulfamethazine (SMZ), and sulfadimethoxine (SDM). The method includes extraction of the product with phosphate buffer, centrifugation of the diluted product, and application of a portion of the extract onto a polymeric solid-phase extraction cartridge. The cartridge is washed with water, and the sulfonamides are eluted with methanol. After evaporation, the residue is dissolved in 0.1% formic acid solution, and the solution is filtered before analysis by LC/MS/MS. The LC/MS/MS program involved a series of time-scheduled selected-reaction monitoring transitions. The transitions of MH+ to the common product ions at m/z 156, 108, and 92 were monitored for each residue. In addition, SMZ and SDM had a fourth significant and unique product ion transition that could be measured. Validation was performed with control and fortified-control condensed bovine milk with 2.5, 5, and 10 ppb sulfonamides. This method was applied to imported flavored and unflavored condensed milk and cream cheese bars. The presence of STZ and SMZ residues was confirmed in 3 out of 6 products.
U.S. Food and Drug Administration, PO Box 25087, Denver, CO 80225, USA.
Susan B
SB
Clark
Sherri B
SB
Turnipseed
Mark R
MR
Madson
Jeffrey A
JA
Hurlbut
Laura R
LR
Kuck
John N
JN
Sofos
D000818:Animals; D002417:Cattle; D002611:Cheese / Q000032:analysis; D002852:Chromatography, Ion Exchange / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination; D005561:Formates / Q000737:chemistry; D007477:Ions; D008892:Milk / Q000378:metabolism; D010710:Phosphates / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013412:Sulfadimethoxine / Q000032:analysis*; D013418:Sulfamethazine / Q000032:analysis*; D000077589:Sulfathiazole; D013432:Sulfathiazoles / Q000032:analysis*; D013997:Time Factors
D005561:Formates; D007477:Ions; D010710:Phosphates; D013432:Sulfathiazoles; C030544:formic acid; D013412:Sulfadimethoxine; D013418:Sulfamethazine; D000077589:Sulfathiazole