Determination of 184 Pesticide Residues in Tobacco by Gas Chromatography-Quadrupole Time of Flight Mass Spectrometry
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摘要: 采用滤头式固相萃取前处理方法，结合气相色谱-四级杆飞行时间质谱（GC-QTOF/MS）检测技术，建立了烟草中184种农药残留的快速筛查和定量测定方法。通过单因素结合Box-Behnken响应面优化试验考察了溶剂用量，加水量及净化量对目标农药回收率的影响。最终确定了烟草样品最佳前处理方法为，15 mL乙腈提取，震荡离心后移取1 mL上清液通过Cleanert NANO净化柱净化，平行浓缩近干后，以0.5 mL丙酮-正己烷（1/1，V/V）进行溶剂置换，GC-QTOF/MS进行检测。结果表明，184种农药在范围内线性关系良好；在0.05、0.25、0.5 μg/g添加水平下，除部分农药回收率较低外，平均回收率分别为62.05%~122.19%、65.18%~120.21%和68.55%~119.41%；相对标准偏差（RSD）范围分别为0.16%~14.04%、0.15%~12.06%和0.03%~14.92%（n=3）；在0.05、0.1、0.5 μg/g添加浓度下，定性筛查软件检出农药的比例分别为71.74%、92.39%和98.91%。该方法操作简便，耗时短，准确性好，能够满足烟草中多农药残留定性和定量检测的要求，具有实际应用价值。
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关键词:
- 滤头式固相萃取 /
- 气相色谱-四级杆飞行时间质谱 /
- 响应面法 /
- 烟草 /
- 农药残留
Abstract: An analytical method for rapid screening of 184 pesticide residues in tobacco was established based on filter solid phase extraction method by gas chromatography-quadrupole time of flight mass spectrometry (GC-QTOF/MS). Single factor examination combined with the Box-Behnken response surface analysis experiments was used to investigate the effects of solvent volume, water volume and purification volume on the recovery of target pesticides. The optimal sample preparation procedure was as follows:the tobacco sample was extracted with 15 mL acetonitrile. After shaking and centrifugation, 1 mL supernatant was cleaned up by Cleanert NANO purification columns. After dried by parallel concentrator, the extract residues were reconstituted with n-hexane-acetone(1/1,V/V) and then detected by GC-QTOF/MS. The linearity of the method was good. At the addition levels of 0.05, 0.25 and 0.5 μg/g, the average recovery rates were 62.05% to 122.19%, 65.18% to 120.21% and 68.55% to 119.41%, except for some pesticides. The relative standard deviation (RSD) were 0.16% to 14.04%, 0.15% to 12.06% and 0.03% to 14.92% (n=3). At the addition levels of 0.05, 0.25 and 0.5 μg/g, the proportion of pesticides detected by the workflow software was 71.74%, 92.39% and 98.91%, respectively. The convenient, rapid and accurate method can be applied for qualitative and quantitative detection of multiple pesticide residues in tobacco. -
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