Dai Xuewei, Wei Biwen, Yu Wenjia, Xu Yongwei
Se Pu. 2015 Oct;33(10):1059-64. doi: 10.3724/sp.j.1123.2015.04047.
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 degrees C, 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.
建立了一种采用超高效合相色谱(UPC2)联用光电二极管阵列检测器(PAD)快速测定塑料制品中萘、苊烯、苊、芴、菲、蒽、荧蒽、芘、苯并(a)蒽、 Chrysene、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)苝的方法。18种多环芳烃(PAHs)在大赛璐IB-3手性柱上以二氧化碳为流动相、甲醇/乙腈(25:75,v/v)为流动相添加剂、柱温40℃、背压15.17 MPa的条件下,在不到8.5分钟内成功分离。每种PAH的峰面积与PAH浓度在0.05 - 50 mg/L范围内呈线性相关(r≥0.999 5)。定量限(LOQs)(S/N>10)为0.05 mg/L。样品经甲苯超声辅助萃取后,采用UPC2-PDA进行分析。塑料样品中PAHs的加标回收率为78.3%至117.6%,18种PAHs峰面积的重复性小于5%(RSD,n = 5)。本UPC2-PDA方法具有速度快、分辨率高、有机试剂消耗低等优点。