色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1059-1064.DOI: 10.3724/SP.J.1123.2015.04047

• 研究论文 • 上一篇    下一篇

超高效合相色谱快速分析塑料制品中的18种多环芳烃

戴雪伟1, 卫碧文1, 望秀丽1, 于文佳1, 徐永威2   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 沃特世科技有限公司, 上海 201206
  • 收稿日期:2015-04-28 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 望秀丽

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

DAI Xuewei1, WEI Biwen1, WANG Xiuli1, YU Wenjia1, XU Yongwei2   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Waters Technologies Corporation, Shanghai 201206, China
  • Received:2015-04-28 Online:2015-10-08 Published:2012-05-09

PDF

113

被引次数

12

摘要：

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。

关键词: 超高效合相色谱, 多环芳烃, 二极管阵列检测器, 塑料制品

Abstract:

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.

Key words: photodiode array detector (PDA), plastic products, polycyclic aromatic hydrocarbons (PAHs), ultra performance convergence chromatography (UPC2)

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