四通道色谱分离仪净化/气相色谱-质谱法测定烟叶中的多环芳烃  被引量:6

Determination of 16 Polycyclic Aromatic Hydrocarbons in Tobacco( Nicotiana Tabacum L.) by Four-channel Chromatograph Purification Coupled with Gas Chromatography-Mass Spectrometry

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作  者:马军[1,2,3] 滕应[2] 陆引罡[1] 甘信宏 任文杰[2] 马文亭[2] 

机构地区:[1]贵州大学农学院,贵州贵阳550025 [2]中国科学院南京土壤研究所土壤环境与污染修复重点实验室,江苏南京210008 [3]铜仁学院材料与化学工程学院,贵州铜仁554300

出  处:《分析测试学报》2016年第8期968-973,共6页Journal of Instrumental Analysis

基  金:环保公益性行业科研专项项目(201109018)

摘  要:建立了同时检测新鲜烟叶中16种多环芳烃(PAHs)的四通道色谱分离仪净化/气相色谱-质谱(GC-MS)分析方法。样品经二氯甲烷索氏提取,四通道色谱分离仪净化,GC-MS选择离子监测模式(SIM)测定和外标法定量,重点考察了新鲜烟叶提取液的分离净化条件。结果表明:16种PAHs类化合物在10~1 000μg/kg范围内定量离子的峰面积与质量浓度呈较好的线性关系(r〉0.99)。仪器检出限(LOD)为0.35~1.75μg/kg,方法检出限(MDLs)为1.01~2.87μg/kg。在10,50,200μg/kg 3个浓度水平下的加标回收率为81.0%~107.8%,相对标准偏差(RSD,n=6)为2.7%~8.0%。该方法简便、快捷、可操作性强、应用范围广,适合于烟草等作物中PAHs类化合物的分析检测。A method for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) in tobacco by four-channel chromatograph purification coupled with gas chromatography - mass spectrometry( GC -MS) was developed. The tobacco samples were extracted by the method of soxhlet extraction with dichloromethane, and the extract was cleaned with four-channel purification chromatograph. The eluent were determined by GC -MS in SIM mode, and quantitated by a method of external standard. The procedure of separation and purification for fresh tobacco extraction was op- timized. The results indicated the calibration curves of 16 PAHs had good linear relationships in the range of 10- 1 000 μg/kg(r 〉 0.99). The detection of limits(LODs) and method detection limits (MDLs) were 0.35 - 1.75 μg/kg and 1.01 - 2. 87 μg/kg, respectively. The recoveries at three spiked concentration levels were in the range of 81.0% - 107.8% with relative standard deviations ( RSD, n = 6) of 2.7% - 8.0%. The method is suitable for the determination of PAHs in tobacco or other crops with easy operation, rapidness, high repeatability and strong practicability.

关 键 词:四通道色谱分离仪 气相色谱-质谱 多环芳烃 净化 烟叶 

分 类 号:O657.63[理学—分析化学] O625.15[理学—化学]

 

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