Interlaboratory study of LC-UV and LC-MS methods for the simultaneous determination of deoxynivalenol and nivalenol in wheat.
To evaluate LC methods with UV or MS detection for simultaneous analysis of deoxynivalenol (DON) and nivalenol (NIV) in wheat, an interlaboratory study was conducted in 11 laboratories. DON and NIV were purified using a multifunctional column, and their concentrations were determined using LC-UV or LC-MS(/MS). No internal standards were used. Three fortified wheat samples (0.1, 0.5 and 1 mg/kg), one naturally contaminated wheat sample, and one blank wheat sample were used. The recoveries ranged from 90% to 110% for DON and from 76% to 83% for NIV. For DON, the relative standard deviations for repeatability (RSDr) ranged from 1.1% to 7.6%. The relative standard deviations for reproducibility (RSDr) ranged from 7.2% to 25.2%. For NIV, the RSDr ranged from 2.0% to 10.7%, and the RSDr ranged from 7.0% to 31.4%. Regardless of sample and detector, the HorRat values for DON and NIV ranged from 0.4 to 1.4. Both LC-UV and LC-MS(/MS) methods were considered to be suitable for application as an official method.
Food and Agricultural Materials Inspection Center, Sendai, Japan. kouji_aoyama@nm.famic.go.jp
Koji
K
Aoyama
Hajime
H
Akashi
Naoki
N
Mochizuki
Yuji
Y
Ito
Takashi
T
Miyashita
Soohyung
S
Lee
Motoki
M
Ogiso
Mamoru
M
Maeda
Shigemi
S
Kai
Hiroki
H
Tanaka
Hiroko
H
Noriduki
Hisaaki
H
Hiraoka
Toshitsugu
T
Tanaka
Eiichi
E
Ishikuro
Yoshinori
Y
Itoh
Toshihiro
T
Nagayama
Masahiro
M
Nakajima
Shigehiro
S
Naito
Yoshiko
Y
Sugita-Konishi
D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D014255:Trichothecenes / Q000032:analysis*; D014908:Triticum / Q000737:chemistry*; D014466:Ultraviolet Rays
D014255:Trichothecenes; C038405:nivalenol; C007262:deoxynivalenol