A liquid-liquid extraction combined with derivatization and gas chromatography-mass spectrometry (GC-MS) method was developed for the rapid determination of C4-C9 alkylphenols (4-tert-butylphenol, 4-n-butylphenol, 4-n-pentylphenol, 4-n-hexylphenol, 4-n-heptylphenol, 4-n-octylphenol, 4-tert-octylphenol, 4-n-nonylphenol and 4-nonylphenol) and bisphenol A in the environmental water. The extraction solvent, extraction time, solvent volume, acidity, salt content and the distillation degree were optimized. After drying and dehydration, the extract was derivatized, detected by GC-MS and quantified by internal standard method. After the dehydration, the extract was derivatized with BSTFA, detected by GC-MS and quantified by internal standard method. The results showed that the relative standard deviations of the relative response factors of the target compounds were less than 20%, the method detection limits were 0.002 µg/Lཞ0.006 µg/L, the relative standard deviations of the three spiked levels were 0.67%ཞ13.7%, and the average recoveries of the actual water samples were 68.0%ཞ122%. The method precision and accuracy were good. The method is simple, rapid, accurate, stable and reliable, which is suitable for the detection of target in water. The contents of C4-C9 alkylphenols and bisphenol A in groundwater, surface water, sewage, waste water and sea water samples in Dongying City located at the Yellow River Estuary were determined by this method. The results showed that the contents of 4-nonylphenol and bisphenol A in these samples were lower than the home and abroad requirements.
A liquid-liquid extraction combined with derivatization and gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of C4-C9 alkylphenols (APs, included 4-tert-butylphenol, 4-n-butylphenol, 4-n-pentylphenol, 4-n-hexylphenol, 4-n-heptylphenol, 4-n-octylphenol, 4-tert-octylphenol, 4-n-nonylphenol and 4-nonylphenol) and bisphenol A (BPA) in environmental water. The extraction solvent, extraction number, extraction time, extraction solvent volume, pH value, salt content, concentration degree and derivatization time were optimized. The target compounds were quantified by internal standard method. Results showed that the optimal extraction number, time, solvent volume, pH value and salt content were 2, 5 min, 30 ml, about 2 and 5 g, respectively, and derivatization time was 1 h at room temperature. Dichloromethane was selected as the extraction solvent and was concentrated to 0.5 mL in the process of concentration. The developed method was validated and showed good linearity (R2 > 0.995), low limit of detection (LOD, 0.002 µg/L–0.006 µg/L), and excellent recovery (68.0 %–122 %) and low relative standard deviation (0.67 %–13.7 %). The developed method was finally applied to groundwater, surface water, seawater and sewage samples in Dongying City located at Yellow River Estuary and some of these target compounds were detected. The measured values of 4-nonylphenol and BPA in these water samples were below their restrictive values of relevant directives at home and abroad.
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