| Bisphenol A(BPA)and its substitutes bisphenol S(BPS)and bisphenol F(BPF)are mainly used in the manufacture of plastic raw materials,and are widely used in the production of polycarbonate plastics,epoxy resin and thermal paper.Because of BPA and its substitutes can be readily released during production,usage and disposal,resulting in their ubiquitous occurrence in the environment.BPA and its substitutes have been found in different environmental media,such as water,soil,sediment,sludge,and in human food and urine.Toxicological experiments have shown that BPA and its substitutes can induce endocrine disruption and physiological toxicity.Due to their toxicity and prevalence in the environment,BPA and its substitutes have impact on human health.Therefore,the establishment of detection and analysis methods for trace BPA and its substitutes in environmental samples is of great significance to better understand its exposure level in the environment and analyze its ecological risk.The present work optimized the sample pretreatment and instrumental detection and analysis conditions and established the detection and analysis methods of trace BPA and its substitutes in environmental samples(water,soil and sediment).The main results are as follows:1.High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was used to determine BPA and its substitutes,and the detection conditions were optimized.The optimal mother ion charge ratios(m/z)of BPA,BPS and BPF were 227.2,249.0 and 199.0,and methanol/water(80:20)was used as the mobile phase for isocratic elution.The optimal ion source temperature and atomizer temperature were 150℃ and 350℃,and the detection time was 7 min.2.SPE was used for pretreatment of water samples.The optimal conditions were as follows:Oasis HLB cartridge solid phase extraction column was selected,the flow rate was 5 mL·min-1,and 15 mL methanol was used for elution.Under the three concentration levels(0.40,1.00and 4.00 ng·mL-1),the recoveries of BPA,BPS and BPF in water samples were85.74±1.80%~109.78±3.05%,the variation coefficients were 0.80~8.19%,and the detection limit was 0.01 ng·mL-1.3.ASE was used for the pretreatment of soil and sediment samples.The extraction temperature was 100℃,the extraction time was 8 min,and the cycle was two times.At three spiked levels(1.25,2.50 and 5.00 ng·g-1),the recoveries of BPA,BPS and BPF in soil were84.96±1.50%~105.86±5.41%,and the variation coefficients were 0.32~9.79%.The recoveries of BPA,BPS and BPF in sediment were 84.31±6.65%~106.36±6.88%,and the coefficient of variation was 1.30~7.89%.The minimum detection limits of soil and sediment were 0.09 and0.12 ng·g-1.4.The optimized detection method was used to detect the drinking water samples sold in the market,and a very small amount of BPA,BPS and BPF could be detected.The detection concentrations of BPA,BPS and BPF in surface water of Xiaoqing River(118.93°E,37.24°N)were 0.18,0.23 and 0.06 ng·mL-1,respectively.In the soil and sediment of Daicunba in Taian(116.55°E,35.89°N),BPA,BPS and BPF were detected with the concentration ranges of0.23~0.66 ng·g-1and 0.24~1.28 ng·g-1,respectively. |