作者：陈冰¹, 肖维毅¹, 尧珍玉¹, 衣志民¹, 徐兰兰¹, 闫洪喜², 何雪峰¹

作者单位：1. 云南瑞升烟草技术(集团)有限公司, 云南 昆明 650106;
2. 浙江中烟工业有限责任公司, 浙江 杭州 310008

关键词：磁性多壁碳纳米管;磁固相萃取;苯并[a]芘;气相色谱-质谱联用

摘要：

建立以磁性多壁碳纳米管(Fe3O4/MWCNTs)作为磁固相萃取吸附剂,气相色谱-质谱联用检测食用油中苯并[a]芘(BaP)的方法。实验优化萃取时间、洗脱溶剂的种类和用量、洗脱时间等影响萃取效率的主要参数。最佳样品处理条件为:萃取时间5 min、4 mL甲苯作为洗脱剂超声洗脱3 min。在最佳条件下,该方法具有较高的准确性和灵敏度,其回收率为95.3%~100.5%,检出限(3倍信噪比)为0.15g/L。检测市售食用油中的BaP时,实际样品加标回收率为77.2%~89.1%,相对标准偏差为1.1%~6.0%,检出限为0.19%~0.29g/L,该方法操作简便、耗时短、有毒试剂用量少、准确灵敏。

Magnetic multi-walled carbon nanotubes as a solid phase extraction adsorbent for the determination of benzo(a) pyrene in cooking oil by gaschromatography-mass spectrometry

CHEN Bing¹, XIAO Weiyi¹, YAO Zhenyu¹, YI Zhimin¹, XU Lanlan¹, YAN Hongxi², HE Xuefeng¹

1. Yunnan Reascend Tobacco Technology(Group)Co., Ltd., Kunming 650106, China;
2. China Tobacco Zhejiang Industrial Co., Ltd., Hangzhou 310008, China

Abstract: This paper is related to a method that magnetic multi-walled carbon nanotubes(Fe₃O₄/MWCNTs) were used as solid-phase extraction adsorbents for the determination of benzo(a) pyrene(BaP) in cooking oil by gas chromatography-mass spectrometry(GC-MS). The main parameters affecting the extraction efficiency were optimized, such as extraction time and variety, dosage and desorption time of desorption solvent. The best conditions of sample treatment were as follows:extraction time is set to 5 min, and ultrasonic desorption time is set to 3 min using 4 mL methylbenzene as desorption solvent. Under the above conditions, the extraction efficiency was ranging from 95.3% to 100.5% with relative standard deviation less than 3%. The limit of detection(S/N=3) for BaP was 0.15μg/L. This method was used for analyzing the cooking oil and no BaP detected. The standard recovery rate was between 77.2% and 89.1% for 6 spiked samples and the relative standard deviation was between 1.1% and 6.0%. It was sensitive when the detection limit(S/N=3) was between 0.19μg/L and 0.29μg/L. This method is simple and fast, accurate and sensitive, and capable of handling large amounts of samples.

Keywords: magnetic multi-walled carbon nanotube;magnetic solid-phase extraction;benzo(a) pyrene;gas chromatography-mass spectrometry

2015, 41(11): 44-49  收稿日期: 2015-03-27;收到修改稿日期: 2015-04-30

基金项目: 

作者简介: 陈冰(1989-),男,云南昆明市人,硕士,主要从事分析化学方面的研究。

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