Chinese Journal of Chromatography, Год журнала: 2023, Номер 41(11), С. 1021 - 1029

Опубликована: Ноя. 1, 2023

Organophosphorus flame retardants (OPFRs) have emerged as good alternatives to brominated retardants, the use of which is globally restricted. In this study, a screening method based on QuEChERS-gas chromatography-quadrupole time-of-flight mass spectrometry (GC-Q-TOF/MS) was established for determination 21 OPFRs in rice. First, full scan (scanning range, m/z 50-450) performed with mixed standard solution (0.1 μg/g) by GC-Q-TOF/MS. The fragmentation pathways these were then investigated explore their cleavage fragments, interrelationships among and possible modes alkylated, chlorinated, aromatic OPFRs. retention times, isotopic abundance ratios, molecular formulas characteristic fragments well exact compounds obtained establish spectral library Rice samples extracted purified QuEChERS method, 0.5% formate acetonitrile used extraction solvent; 4 g magnesium sulfate, 1 sodium chloride, 0.5 disodium hydrogen citrate, citrate extraction-salt combination; 50 mg primary secondary amine (PSA), octadecylsilane (C18), 150 sulfate purification materials. chromatographic separation completed within 16 min under optimized temperature program conditions DB-5MS UI column. parameters optimized, following conditions: number fragment ions ≥2; accurate window=±2×10-5 (±20 ppm); time deviation=±0.2 min, ion deviation<20%. developed applied samples. results indicated that matrix interference greatly reduced decreasing window, thereby improving signal-to-noise ratio analytes. targets from background noise using deconvolution software, improved match between target library. detection rates alkyl increased 22% 25%, respectively, when spiking level 2 10 ng/g. Among chlorinated OPFRs, only tris(2-chloroisopropyl) phosphate (TCIPP) not detected at ng/g, indicating could be identified even low concentrations. matched those home-made well, practical application rice different regions China. A total 11 detected, trimethyl (TMP), tri-iso-butyl (TiBP), tris(3,5-dimethylphenyl) (T35DMPP) had highest rates. These indicate three are widely can easily come into contact through various routes. Differences types actual may related produced local factories. GC-Q-TOF/MS helpful identification complex

Язык: Английский