Selective Solid Phase Extraction of Nonylphenol and Bisphenol A in Environmental and Food Samples Using Double_Molecularly Imprinted Polymer Microsphere / 分析化学

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.

Simultaneous Determination of Nonylphenol, Octylphenol and Bisphenol A in Textiles and Food Packaging Materials by Liquid Chromatography Tandem Mass Spectrometry / 分析化学

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.