title: Determination of perchlorate anion in foods by ion chromatography-tandem mass spectrometry.
abstract: A rapid, sensitive, and specific method was developed for determining perchlorate anion in lettuce, cantaloupe, bottled water, and milk. A test portion of chopped crop homogenate was extracted with diluted nitric acid and filtered. Milk proteins were precipitated with acetonitrile, and the supernatant, after centrifugation, was cleaned up on a graphitized carbon solid-phase extraction column. Water samples were analyzed directly. All test solutions were syringe filtered and mixed with an 18O4-labeled perchlorate internal standard before ion chromatography-tandem mass spectrometry. A strong anion exchange column eluted with 100 mM ammonium acetate in 50:50 (v/v) acetonitrile/water was interfaced via electrospray ionization to a triple stage quadrupole mass spectrometer operated in the negative ion mode. The labeled internal standard corrected for any sample matrix effects on measured signals. Four parent-to-product ion transitions, for loss of oxygen, were monitored for native and 18O4-labeled perchlorate anion, respectively: 35Cl-perchlorate, m/z 99 --> 83 and 107 --> 89; 37Cl-perchlorate, m/z 101 --> 85 and 109 --> 91. The limit of quantitation was 1.0 microg/kg in lettuce, 2.0 microg/kg in cantaloupe, 0.50 microg/L in bottled water, and 3.0 microg/L in milk. Native perchlorate was recovered from fortified test portions in the range 93-107% for lettuce, 107-114% for cantaloupe, 100-115% for bottled water, and 99-101% for milk.
authors.affiliation: Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, USA. Alex.Krynitsky@cfsan.fda.gov
authors.forename: Alexander J
authors.initials: AJ
authors.lastname: Krynitsky
authors.forename: Richard A
authors.initials: RA
authors.lastname: Niemann
authors.forename: David A
authors.initials: DA
authors.lastname: Nortrup
mesh_terms: D000818:Animals; D002417:Cattle; D002852:Chromatography, Ion Exchange / Q000379:methods*; D028463:Cucumis melo / Q000737:chemistry; D005504:Food Analysis / Q000379:methods*; D018545:Lactuca / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods*; D008892:Milk / Q000737:chemistry; D010472:Perchlorates / Q000032:analysis* / Q000737:chemistry*; D012680:Sensitivity and Specificity; D014867:Water / Q000737:chemistry
chemical_list: D010472:Perchlorates; D014867:Water