Xiu X.,Qingdao University of Science and Technology |
Xiu X.,Technical Center for Inspection |
Luo X.,Technical Center for Inspection |
Niu Z.,Technical Center for Inspection |
And 5 more authors.
Chinese Journal of Chromatography (Se Pu) | Year: 2013
A method of high performance liquid chromatography-linear ion trap/Orbitrap high resolution mass spectrometry (HPLC-LTQ/Orbitrap MS) was used to screen and confirm carci-nogenic dyes in textiles. The analytes were extracted from textile samples with pyridine/water (1/1, v/v) in a water bath under controlled conditions (95 °C 150 r/min), and then filtered with a 0.22 μm polytetrafluoroetylene (PTFE) membrane. The eluates were separated on a CAPCELL PAK C18 column (100 mm ×2.0 mm, 5 μm) using gradient elution with acetonitrile/5 mmol/L ammonium acetate aqueous solution containing 0.01% formic acid ( in positive mode) and acetonitrile/5 mmol/L ammonium acetate aqueous solution (in negative mode), and finally detected by HPLC-LTQ/Orbitrap MS in ESI modes. Full scan experiments were per-formed over the range of m/z 200 - 800. The screening and quantitative analysis were carried out by the accurate mass of quasi-molecular ion and the peak area in extracted chromatogram with accurate mass, respectively. The confirmatory analysis for target compounds was per-formed with the retention time and qualitative fragments obtained by data-dependent scan mode. Under the optimal conditions, nine carcinogenic dyes were routinely detected with mass accuracy below 5 ×10-6(5 ppm), and good linearities were provided in their respective linear ranges with correlation coefficients higher than 0.99. The limits of detection were in the range of 0.125 -25 mg/kg. The average recoveries at three spiked levels were in the range of 62.13% -116.28% with the relative standard deviations (RSDs) lower than 15%. The proposed method was applied to screen and confirm the nine carcinogenic dyes in textile samples. It is convenient and reliable.