RESUMEN
Double template molecularly imprinted polymer ( D_MIP) was prepared by emulsion polymerization method using the nonylphenol (NP), bisphenol A (BPA) as templates, α_methyl methacrylate(MAA) as functional monomer. Then using the D_MIP as solid phase extraction materials, a method based on double_molecularly imprinted solid phase extraction coupled with high performance liquid chromatographic fluorescence detection was developed for the determination of trace NP and BPA from environmental and food samples. The D_MIP was characterized by Fourier transform infrared spectroscopy ( FT_IR ) and adsorption experiments. The results showed that the saturated adsorption capacity of the D_MIP for NP and BPA was 73. 3 and 97. 5 mg/g, respectively, and the relative selectivity coefficient was 2. 2 and 1. 7, respectively. Moreover, the conditions affecting extraction efficiency, such as washing conditions and desorption conditions were optimized. Under the optimal conditions, there was a good linear correlation in the concentration range of 0. 01-2. 3 mg/L with correlation coefficients (R2) greater than 0. 998 for NP and BPA. The detection limits ( S/N=3) were 0. 001 and 0. 002 mg/L. The proposed method was applied to determine NP and BPA in river water, beer and crucian carp samples. The recoveries of NP and BPA were in the range of 86. 4%-99. 1%with the relative standard deviation less than 6 . 2%. This method has good selectivity and high sensitivity and shows good prospects for the application in the enrichment and separation of NP and BPA in real samples.
RESUMEN
A comprehensive analytical method based on liquid chromatography tandem mass spectrometry has been developed for the determination of nonylphenol, octylphenol and bisphenol A in textiles and food packaging) materials. Various textile and food packaging material samples were extracted under the conditions of 10.3 MPa and 120 ℃ by accelerated solvent extraction method with two static cycles using ethanol as the extraction) solvent. The extract was cleaned up by Supelclean Envi-Carb solid phase extraction cartridge. Qualitative) and quantitative analyses were carried out for the analytes under the multiple reaction monitoring(MRM) mode after the chromatographic separation on Waters XBridge C_(18))(150 mm×2.1 mm, 3.5 μm) column) with methanol-0.1% NH_4OH gradient elution. The limits of detection(LODs) for alkylphenol, octyphenol and bisphenol A were 0.5 μg/kg. The mean recoveries for textile samples at the spiked level of 0.5-10 μg/kg were 86.9%-92.5%, with the relative standard deviation less than 9.1%. The mean recoveries for food packaging material samples at the spiked level of 0.5-10 μg/kg were 87.8%-93.0%, with the relative standard deviation less than 8.8%. The method is accurate, simple, rapid, and adapts to the inspection of nonylphenol, octylphenol and bisphenol A in textiles and food packaging materials.