科研之友
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摘要
The aquicolous organism samples were shelled, stirred and mixed respectively. The dried samples were dried deeper, rubbed and sifted out. The treated sample was extracted by acetone thrice in ultrasonic bath, then mixed the three extracted solutions. Anhydrous Na2SO4 was used to remove water in extract solution and NZ was used to concentrate the solution. The concentrated solution was transferred to Florisil column and the mixture of acetic ester and alkyl (1/5, v/v) was used to elute it. At last, the treated samples were analyzed qualitatively by gas chromatography-electron impact mass spectrometry (GC-EI/MS), and they were quantified by internal standard method. The conditions of pretreatment such as the selection of the extractant, the sorbent, the sorbent activation method and the eluent were optimized. The problem of controlling analysis blank was discussed. The linear correlation coefficient was higher than 0. 9999, the limit of detection was lower than 3. 7 g/L, the recovery values were in the range of 64.1% to 124% and the relative standard deviation of the method was lower than 16.4%. This method was successfully applied to analyze seventeen kinds of phthalates of environmental incretion simultaneously in three kinds of fish(saury, snakehead, curcian), two kinds of seashell (sand snail, oyster), one shellfish (prawn), one cephalopod (octopus), two kinds of plant (kelp, seaweed) and two dried food( dried kelp, dried whitebait). Dimethyl phthalate, diisobutyl phthalate and dibutyl phthalate were determined in all samples. Diethyl phthalate and Di(2-ethyl hexyl) phthalate were determined in many samples. It showed that these five kinds of phthalates had polluted the water in a certain extent.
