建立了一种超高效合相色谱-二极管阵列检测器快速分析塑料制品中萘、苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并(a)蒽、屈艹、苯并(b)荧蒽、苯并(k)荧蒽、苯并(j)荧蒽、苯并(e)芘、苯并(a)芘、茚并(1,2,3-cd)芘、二苯并(a,h)蒽、苯并( g,h,i)!(二萘嵌苯)的方法。以甲苯为溶剂,超声萃取实际塑料制品中的多环芳烃,经超高效合相色谱分析。采用 Daicel IB-3手性色谱柱,以 CO2为流动相,甲醇/乙腈(25:75,v/v)为流动相助溶剂,在柱温为40℃,背压为15.17 MPa的条件下,18种多环芳烃在8.5 min之内实现基线分离。18种多环芳烃的线性范围为0.05~50 mg/L( r≥0.9995),定量限( S/N>10)为0.05 mg/L。加标回收率为78.3%~117.6%,相对标准偏差( RSD,n=5)小于5%。该方法具有分析速度快、分离效率高、节约有机溶剂的优点。
A method for rapid determination of naphthalene,acenaphthylene,acenaphthene, fluorene,phenanthrene,anthracene,fluoranthene,pyrene,benzo( a)anthracene,chrysene, benzo( b)fluoranthene,benzo( k)fluoranthene,benzo( j)fluoranthene,benzo( e)pyrene,benzo (a)pyrene,indeno(1,2,3-cd)pyrene,dibenzo(a,h)anthracene,benzo(g,h,i)perylene in plastic products by ultra performance convergence chromatography( UPC2)coupled photodi-ode array detector( PAD)was developed. The 18 polycyclic aromatic hydrocarbons( PAHs) were successfully separated in less than 8. 5 min on a Daicel IB-3 chiral column with a mobile phase of CO2,the mobile-phase additive of methanol/acetonitrile(25:75,v/v)at column tem-perature of 40 ℃,and a back pressure of 15. 17 MPa. There was a linear correlation between peak area and PAH concentration in the range of 0. 05-50 mg/L( r≥0. 999 5)for each PAH. The limits of quantification ( LOQs )( S/N>10 ) were 0. 05 mg/L. After ultrasonic-assisted extraction in toluene,the sample was analyzed by UPC2-PDA. The recoveries of PAHs spiked in plastic samples were from 78. 3% to 117. 6%,and the repeatabilities of peak areas for the 18 PAHs were less than 5%(RSD,n=5). The present UPC2-PDA method has the advantages of rapid speed,high resolution,and low organic reagent consumption.
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