title: A liquid chromatography-tandem mass spectrometry method for the detection of economically motivated adulteration in protein-containing foods.
abstract: A new analytical method was developed to determine the presence of six (6) compounds with the potential to be used in economic adulteration to enhance the nitrogen content in milk products and bulk proteins. Residues were extracted from the matrix with 2% formic acid, after which acetonitrile (ACN) was added to induce precipitation of the proteins. Extracts were analyzed by liquid chromatography using a ZIC-HILIC column with tandem mass spectrometry (LC-MS/MS) using electrospray ionization (ESI). Single-laboratory method validation data was collected in six matrices fortified at concentrations down to 1.0 μg/g (ppm). Average recoveries and average relative standard deviations (RSD) using spiked matrix calibration standard curves were the following: cyromazine (CY) 95.9% (7.5% RSD), dicyandiamide (DC) 98.1% (5.6% RSD), urea 102.5% (8.6% RSD), biuret (BU) 97.2% (6.6% RSD), triuret (TU) 97.7% (5.7% RSD), and amidinourea (AU) 93.4% (7.4% RSD). This method provides a rapid and effective approach to proactively combat economically motivated adulteration in protein-containing products.
authors.affiliation: United States Food and Drug Administration, Center for Food Safety and Applied Nutrition, College Park, MD, USA. shaun.macmahon@fda.hhs.gov
authors.forename: Shaun
authors.initials: S
authors.lastname: MacMahon
authors.forename: Timothy H
authors.initials: TH
authors.lastname: Begley
authors.forename: Gregory W
authors.initials: GW
authors.lastname: Diachenko
authors.forename: Selen A
authors.initials: SA
authors.lastname: Stromgren
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D005506:Food Contamination / Q000032:analysis* / Q000191:economics; D006146:Guanidines / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D011506:Proteins / Q000032:analysis*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014227:Triazines / Q000032:analysis* / Q000737:chemistry; D014508:Urea / Q000031:analogs & derivatives / Q000737:chemistry
chemical_list: D006146:Guanidines; D011506:Proteins; D014227:Triazines; D014508:Urea; C028704:cyromazine; C004711:dicyandiamido; C011907:melamine