title: Simultaneous determination of seven anticoagulant rodenticides in agricultural products by gel permeation chromatography and liquid chromatography-tandem mass spectrometry.
abstract: A sensitive and reliable method for the simultaneous determination of hydroxycoumarin-type (brodifacoum, bromadiolone, coumatetralyl, and warfarin) and indandione-type (chlorophacinone, diphacinone, and pindone) rodenticides in agricultural products by gel permeation chromatography (GPC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The procedure involved extraction of the rodenticides from samples with acetone, followed by liquid-liquid partitioning with hexane/ethyl acetate (1:1, v/v) and 10% sodium chloride aqueous solution, then cleanup using GPC, and finally, analysis using LC-MS/MS. High recoveries from the GPC column were obtained for all rodenticides tested using a mobile phase of acetone/cyclohexane/triethylamine (400:1600:1, v/v/v). An ODS column, which contains low levels of metal impurities, gave satisfactory peak shapes for both hydroxycoumarin- and indandione-type rodenticides in the LC-MS/MS separation. The average recoveries of rodenticides from eight agricultural foods (apple, eggplant, cabbage, orange, potato, tomato, brown rice, and soybean) fortified at 0.0005-0.001 mg/kg ranged from 76 to 116%, except for bromadiolone in orange (53%) and diphacinone in soybean (54%), and the relative standard deviations ranged from 1 to 16%. The proposed method effectively removed interfering components, such as pigments and lipids, and showed high selectivity. In addition, the matrix effects were negligible for most of the rodenticide/food combinations. The results suggest that the proposed method is reliable and suitable for determining hydroxycoumarin- and indandione-type rodenticides in agricultural products.
authors.affiliation: a Division of Foods, National Institute of Health Sciences , Tokyo , Japan.
authors.forename: Shizuka
authors.initials: S
authors.lastname: Saito-Shida
authors.affiliation: a Division of Foods, National Institute of Health Sciences , Tokyo , Japan.
authors.forename: Satoru
authors.initials: S
authors.lastname: Nemoto
authors.affiliation: a Division of Foods, National Institute of Health Sciences , Tokyo , Japan.
authors.forename: Rieko
authors.initials: R
authors.lastname: Matsuda
authors.affiliation: a Division of Foods, National Institute of Health Sciences , Tokyo , Japan.
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Akiyama
mesh_terms: D015110:4-Hydroxycoumarins / Q000032:analysis*; D000925:Anticoagulants / Q000032:analysis*; D002850:Chromatography, Gel; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods; D018556:Crops, Agricultural / Q000737:chemistry*; D004784:Environmental Monitoring; D007189:Indans / Q000032:analysis*; D010630:Phenindione / Q000032:analysis*; D012378:Rodenticides / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D015110:4-Hydroxycoumarins; D000925:Anticoagulants; D007189:Indans; D012378:Rodenticides; D010630:Phenindione
keywords: Rodenticide; agricultural products; gel permeation chromatography; liquid chromatography; tandem mass spectrometry