title: Determination of a metabolite of nifursol in foodstuffs of animal origin by liquid-liquid extraction and liquid chromatography with tandem mass spectrometry.
abstract: An analytical method has been developed for the detection of a metabolite of nifursol, 3,5-dinitrosalicylic acid hydrazide, in foodstuffs of animal origin (chicken liver, pork liver, lobster, shrimp, eel, sausage, and honey). The method combines liquid chromatography and tandem mass spectrometry with liquid-liquid extraction. Samples were hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde at 37°C for 16 h. The solutions of derivatives were adjusted to pH 7.0-7.5, and the metabolite was extracted with ethyl acetate. 3,5-Dinitrosalicylic acid hydrazide determination was performed in the negative electrospray ionization method. Both isotope-labeled internal standard and matrix-matched calibration solutions were used to correct the matrix effects. Limits of quantification were 0.5 μg/kg for all samples. The average recoveries, measured at three concentration levels (0.5, 2.0, and 10 μg/kg) were in the range of 75.8-108.4% with relative standard deviations below 9.8%. The developed method exhibits a high sensitivity and selectivity for the routine determination and confirmation of the presence of a metabolite of nifursol in foodstuffs of animal origin.
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai, China.
authors.forename: Chuanxian
authors.initials: C
authors.lastname: Wang
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai, China.
authors.forename: Li
authors.initials: L
authors.lastname: Qu
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai, China.
authors.forename: Xia
authors.initials: X
authors.lastname: Liu
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai, China.
authors.forename: Chaomin
authors.initials: C
authors.lastname: Zhao
authors.affiliation: Food Inspection Center of Shenzhen Entry-Exit Inspection and Quarantine, Shenzhen, China.
authors.forename: Fengjuan
authors.initials: F
authors.lastname: Zhao
authors.affiliation: Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou, China.
authors.forename: Fuzhen
authors.initials: F
authors.lastname: Huang
authors.affiliation: Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou, China.
authors.forename: Zhenou
authors.initials: Z
authors.lastname: Zhu
authors.affiliation: Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou, China.
authors.forename: Chao
authors.initials: C
authors.lastname: Han
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid; D005504:Food Analysis / Q000379:methods*; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction; D008460:Meat / Q000032:analysis*; D008461:Meat Products / Q000032:analysis*; D009581:Nitrofurans / Q000032:analysis* / Q000737:chemistry; D013552:Swine; D053719:Tandem Mass Spectrometry
chemical_list: D009581:Nitrofurans; C032119:nifursol
keywords: foodstuffs; liquid chromatography; metabolites; nifursol; tandem mass spectrometry