雾非雾
第3楼2011/10/27
ACCESSION: WA000054
RECORD_TITLE: Chromafenozide; LC-ESI-QQ; MS2; CE:30 V; [M+H]+
DATE: 2011.05.06 (Created 2007.08.01)
AUTHORS: Nihon Waters K.K.
LICENSE: Copyright 2007-2011 Nihon Waters K.K.
CH$NAME: Chromafenozide
CH$COMPOUND_CLASS: N/A
CH$FORMULA: C24H30N2O3
CH$EXACT_MASS: 394.22564
CH$SMILES: Cc(c3)cc(cc(C)3)C(=O)N(NC(=O)c(c1)c(C)c(C2)c(OCC2)c1)C(C)(C)C
CH$IUPAC: InChI=1S/C24H30N2O3/c1-15-12-16(2)14-18(13-15)23(28)26(24(4,5)6)25-22(27)20-9-10-21-19(17(20)3)8-7-11-29-21/h9-10,12-14H,7-8,11H2,1-6H3,(H,25,27)
CH$LINK: CAS 143807-66-3
AC$INSTRUMENT: QuattroPremier XE, Waters
AC$INSTRUMENT_TYPE: LC-ESI-QQ
AC$MASS_SPECTROMETRY: MS_TYPE MS2
AC$MASS_SPECTROMETRY: ION_MODE POSITIVE
AC$MASS_SPECTROMETRY: COLLISION_ENERGY 30 V
MS$FOCUSED_ION: PRECURSOR_TYPE [M+H]+
MS$FOCUSED_ION: PRECURSOR_M/Z 395.36
MS$DATA_PROCESSING: FIND_PEAK ignore rel.int. < 5
PK$NUM_PEAK: 6
PK$PEAK: m/z int. rel.int.
104 16 16
119 8 8
133 118 118
147 16 16
175 999 999
176 27 27
雾非雾
第5楼2011/10/28
The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 gkg(-1), while the limit of quantification did not exceed 2 gkg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1mgkg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n=5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.
QuEChERS方法(C18、PSA)进行前处理。