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常见饮料和食用油中邻苯二甲酸酯类塑化剂的检测与分析-应用化学专业论文
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Determination and analysis of phthalates plasticizer in common drinks and edible oil
Abstract
Nine kinds of drinks and five kinds of edible oil purchased by the markets, as the research object, were separately stored under 10℃, 20℃ and 30℃, and the fifteen kinds of
PAEs contents in these samples were detected by using gas chromatograph/mass spectrometer (GC/MS). Then, the PAEs contents were monitored irregularly and analyzed the immigration during the expiration date.
First, the separation condition of gel chromatographic column was optimized and the pretreatment conditions of edible oil were built. The pretreatment methods were shown as the follows: (1) Extracted by acetonitrile for four times. (2) Dried by vacuum-rotary evaporation.
(3) Added 2mL cyclohexane and ethyl acetate mixture (V:V=1:1) to dissolve the extract. (4) Seperated the extract with a gel column chromatography and collected effluent from 41mL to 90mL. (5) dried effluent by vacuum-rotary evaporation. (6) added 1mL n-hexane to volume. Besides, in order to obtain precise results, the analysis methods of these plasticizers by GC/MS were also established. GC/MS testing conditions: HP-5MS capillary column,
injection port temperature 280℃, The oven temperature was programmed elevation from
initially 100℃, then increased to 250℃ at 10℃/min,finally reached 280oC at 3℃/min. The experimental results showed that 15 kinds of PAEs appeared good linear, correlation coefficient R was all above 0.999 and the minimum detection limits were between 0.001 and 2.000μg/L.
The sample’s preparation methods had been established by a series of different experimentations, and then we evaluated the methods. The average recoveries of PAEs in drinks are between 69.57% and 112.23%, the relative standard deviations (RSD) from 2.66% to 9.86%. The average recoveries of PAEs in edible oil are between 70.50% and 112.00%, the relative standard deviations (RSD) from 1.59% to 7.54%. The results showed that the methods were
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