Determination of 7B3 residues in cotton plants by liquid chromatography/mass spectrometry.
A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrile-water (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1-100.2%, and the relative standard deviations were <7.5% for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.
Yan
Xiao-Jing
XJ
China Agricultural University, Department of Applied Chemistry, Key Laboratory of Pesticide Chemistry and Application Technology, Beijing 100094, People's Republic of China.
Liang
Xiao-Mei
XM
Xu
Yan-Jun
YJ
Jin
Shu-Hui
SH
Wang
Dao-Quan
DQ
D002498:Centrifugation; D002853:Chromatography, Liquid / Q000379:methods; D005659:Fungicides, Industrial / Q000032:analysis*; D003368:Gossypium / Q000737:chemistry*; D007202:Indicators and Reagents; D007769:Lactams / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods; D012996:Solutions; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D005659:Fungicides, Industrial; D007202:Indicators and Reagents; D007769:Lactams; D012996:Solutions