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真空浓缩-同位素稀释气相色谱-质谱联用法测定辣条中4种多环芳烃

[Determination of 4 polycyclic aromatic hydrocarbons in spicy strips by vacuum concentration coupled with isotope dilution gas chromatography-mass spectrometry].

作者信息

Sha Xianliang, Wu Pinggu, Qin Yanping, Li Gang, Shao Bin, Li Jianlin

机构信息

Changxing County Center for Disease Control and Prevention, Huzhou 313100, China.

Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China.

出版信息

Wei Sheng Yan Jiu. 2020 Jul;49(4):603-612. doi: 10.19813/j.cnki.weishengyanjiu.2020.04.014.

DOI:10.19813/j.cnki.weishengyanjiu.2020.04.014
PMID:32928352
Abstract

OBJECTIVE

A method based on isotope internal standard dilution was established for the determination of four polycyclic aromatic hydrocarbons(PAH4) including chrysene, benzo [a] anthracene, benzo [b] fluoranthene and benzo [a] pyrene in spicy strips sold in the markets.

METHODS

The hot strips were homogenized and the target compounds were extracted with n-hexane, concentrated in vacuum, saponified and purified by solid phase extraction column, then the pretreated samples were separated by DB-EUPAH column(20 m×0. 18 mm, 0. 14 μm), detected by gas chromatography-mass spectrometry(GC-MS)and quantified by internal standard of isotope.

RESULTS

The recoveries of PAH4 in different concentration levels of hot noodles were 91. 0%-103. 5%, and the relative standard deviation(RSD)was 1. 89%-6. 73%(n=6). The detection limit was 0. 30 μg/kg and the quantitative limit was 1. 0 μg/kg. The content of PAH4(sum) in 27 collected samples ranged from 1. 35 μg/kg to 11. 44 μg/kg, and the detection rate was 100%.

CONCLUSION

With less solvent consumption, good purification effect and blank control, the method is simple, rapid and accurate and meets the detecting requirements of PAH4 in hot strips.

摘要

目的

建立一种基于同位素内标稀释法测定市售辣条中包括芘、苯并[a]蒽、苯并[b]荧蒽和苯并[a]芘在内的4种多环芳烃(PAH4)的方法。

方法

将辣条匀浆,目标化合物用正己烷提取,真空浓缩,皂化后经固相萃取柱净化,然后将预处理后的样品用DB-EUPAH柱(20 m×0.18 mm,0.14 μm)分离,采用气相色谱-质谱联用仪(GC-MS)检测,同位素内标法定量。

结果

不同浓度水平的辣条中PAH4的回收率为91.0%103.5%,相对标准偏差(RSD)为1.89%6.73%(n=6)。检出限为0.30 μg/kg,定量限为1.0 μg/kg。所采集的27份样品中PAH4(总量)含量在1.35 μg/kg至11.44 μg/kg之间,检出率为100%。

结论

该方法溶剂消耗少,净化效果好,能有效控制空白,简单快速准确,满足辣条中PAH4的检测要求。

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