Determination of amitraz and 2,4-dimethylaniline residues in honey by using LC with UV detection and MS/MS.
A method for the determination and confirmation of amitraz and its degradation product 2,4-dimethylaniline (2,4-DMA) in honey is reported. Determination of the two compounds was based on HPLC with UV detection and MS/MS (LC-MS/MS) after a liquid-liquid extraction with hexane and isopropyl alcohol. Chromatographic separation was achieved by using a C18 column with a gradient mobile phase consisting of 0.02 M ammonium acetate and ACN. Recoveries for fortified honey ranged from 83.4 to 103.4% for amitraz and from 89.2 to 104.7% for 2,4-DMA with RSD values lower than 11.6% for HPLC and LC-MS/MS methods. LOD was 6 microg/kg for amitraz and 8 microg/kg for 2,4-DMA, while LOQ was 20 microg/kg for amitraz and 25 microg/kg for 2,4-DMA in HPLC method. LOD was 1 microg/kg for amitraz and 2 microg/kg for 2,4-DMA, while LOQ was 5 microg/kg for amitraz and 10 microg/kg for 2,4-DMA in LC-MS/MS method.
Xu
Jin-Zhong
JZ
National Bee-Product Reference Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing, PR China. xujz@jsciq.gov.cn
Miao
Jian-Jun
JJ
Lin
Hong
H
Ding
Tao
T
Zhao
Zhen-Yun
ZY
Wu
Bin
B
Shen
Chong-Yu
CY
Jiang
Yuan
Y
D056810:Acaricides / Q000032:analysis; D000814:Aniline Compounds / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D006722:Honey / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014052:Toluidines / Q000032:analysis*
D056810:Acaricides; D000814:Aniline Compounds; D010573:Pesticide Residues; D014052:Toluidines; C014983:amitraz; C009694:2,4-xylidine