This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile sampl...This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles.展开更多
An effective method was established to determine the content of residual chlorothalonil in textiles by gas chromatography/mass spectrometry-selected ion monitoring coupled with ultrasonic extraction technique. Residua...An effective method was established to determine the content of residual chlorothalonil in textiles by gas chromatography/mass spectrometry-selected ion monitoring coupled with ultrasonic extraction technique. Residual chlorothalonil in textiles was ultrasonically extracted using ethyl acetate as the extraction solvent. The extract was condensed and analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode (GC/MS-SIM). The concentration of chlorothalonil was calibrated by the external standard method. Good linearity existed between the peak area and the mass concentration of chlorothalonil in the mass concentration range from 0.2 μg/mL to 42.8 μg/mL. The equation was A = 95,399ρ ? 50,848, with a correlation coefficient of 0.9999. The limit of detection was 0.1 mg/kg for chlorothalonil. The blank samples were spiked at three concentration levels, and the spiked average recoveries changed from 81.9% to 95.4% while the relative standard deviation (RSD) changed from 1.8% to 5.2%. The proposed method was simple, rapid, sensitive and the limit of detection could meet the limit requirements of relevant regulations. Commercially available textiles were measured by this method, and chlorothalonil at different concentration levels was detected in some samples.展开更多
文摘This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles.
文摘An effective method was established to determine the content of residual chlorothalonil in textiles by gas chromatography/mass spectrometry-selected ion monitoring coupled with ultrasonic extraction technique. Residual chlorothalonil in textiles was ultrasonically extracted using ethyl acetate as the extraction solvent. The extract was condensed and analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode (GC/MS-SIM). The concentration of chlorothalonil was calibrated by the external standard method. Good linearity existed between the peak area and the mass concentration of chlorothalonil in the mass concentration range from 0.2 μg/mL to 42.8 μg/mL. The equation was A = 95,399ρ ? 50,848, with a correlation coefficient of 0.9999. The limit of detection was 0.1 mg/kg for chlorothalonil. The blank samples were spiked at three concentration levels, and the spiked average recoveries changed from 81.9% to 95.4% while the relative standard deviation (RSD) changed from 1.8% to 5.2%. The proposed method was simple, rapid, sensitive and the limit of detection could meet the limit requirements of relevant regulations. Commercially available textiles were measured by this method, and chlorothalonil at different concentration levels was detected in some samples.
