ABSTRACT
A rapid method was developed for the determination of 9 organophosphorous flame retardants ( OPFRs) in textiles by ultra high performance liquid chromatography tandem electrospray ionization mass spectrometry ( UHPLC-MS/MS ) . Analytes in textile samples were extracted in a closed bottle at 50℃ with methanol by ultrasonic extraction for 30 min. And then, the extracted solution was injected after filtration and determined by UHPLC-MS/MS. Target analytes were separated by C18 column and methanol/water containing 5. 0 mmol/L NH4 COOH. The positive electrospray ionization and multiple reaction monitoring mode ( MRM) was utilized. The matrix effect (ME) could be compensated by adjusting the concentration of NH4COOH and the composition of the mobile phase after careful investigation with blank samples. An external standard calibration method was chosen to the quantitative analysis. Under the optimized conditions, method precision represent with relative standard deviations (RSDs) was 5. 2% (TOCP) -12. 5% (TRIS) for cotton, 6. 4%(TBEP)-13. 8% (TRIS) for polyester, and 6. 9% (TDCP) -14. 5% (TEPA) for wool samples. The recoveries for standard addition were in the range of 52 . 5% ( TEPA ) -116 . 4% ( TPP ) . The limits of quantification (LOQ, S/N=10) were between 1. 0 (TBP) and 10. 0 (TRIS) μg/kg.
ABSTRACT
A high sensitive hydride generation ( HG) atomic fluorescence spectrometric system was developed using high current microsecond pulsed hollow cathode lamp ( HCMP-HCL) as the excitation source and its performance was evaluated. Test results confirmed that the excitation source could give out intensive atomic spectral lines. System precision (RSD, n=7) was 1. 1% for arsenic and 1. 4% for selenium. Detection limits (DLs, 3) were 0. 0066 μg/L and 0. 0075 μg/L, respectively. The developed AFS system was proved to have high reliability, low detection limit and remarkable improvement of analysis capability compared with that of commercial AFS instruments.