超高效合相色谱快速分析塑料制品中的18种多环芳烃

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)苝(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。

Determination of 18 polycyclic aromatic hydrocarbons in plastic products by ultra performance convergence chromatography

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 photodiode 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 temperature 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≥0.9995) 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.