张 群,吴南村,刘春华.气相色谱-串联质谱法测定韭菜中的氯氟氰菊酯残留[J].食品安全质量检测学报,2017,8(7):2792-2796 |
气相色谱-串联质谱法测定韭菜中的氯氟氰菊酯残留 |
Determination of cyhalothrin pesticide residues in leek by gas chromatography-tandem mass spectrometry |
投稿时间:2017-04-21 修订日期:2017-07-10 |
DOI: |
中文关键词: 韭菜 氯氟氰菊酯 气相色谱-串联质谱法 |
英文关键词:leek cyhalothrin gas chromatography-tandem mass spectrometry |
基金项目:热带农产品质量安全科技创新团队-北运菜监控项目(1630082017002) |
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中文摘要: |
目的 建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定韭菜中氯氟氰菊酯残留量的分析方法。方法 将韭菜样品的乙腈提取物经石墨化碳黑/氨基混合型固相萃取柱净化、乙腈-甲苯(3:1, V:V)洗脱以及浓缩定容后进行检测。目标化合物经SLB-5MS(30 m×0.25 mm, 0.25 μm)色谱柱分离后, 通过三重串联四级杆多反应监测模式对其进行定性定量分析。结果 在添加水平为0.05~0.50 mg/L(n=5)时, 氯氟氰菊酯的回收率在81.7%~99.1%之间, 相对标准差(RSD)在2.5%~8.7%之间。该方法的线性范围为0.05~0.50 mg/L, 相关系数r2>0.990, 检出限为0.001 mg/kg, 定量限为0.01 mg/kg。结论 该方法能满足韭菜中氯氟氰菊酯残留检测的要求。 |
英文摘要: |
Objective To establish a method for determination of cyhalothrin in leek by gas chromatography- tandem mass spectrometry (GC-MS/MS). Methods The acetonitrile extraction of leek samples was purified by amino hybrid graphitized carbon black/solid phase extraction column, eluted by acetonitrile-toluene (3:1, V:V) and detected after concentration. The target compounds were separated using a SLB-5MS (30 m×0.25 mm, 0.25 μm) chromatographic column, and analyzed qualitatively and quantitatively by triple tandem level 4 pole multiple reaction monitoring mode. Results At addition levels of 0.05~0.50 mg/L (n=5), recovery rates of cyhalothrin were between 81.7%~99.1%, and the relative standard deviations (RSDs) were between 2.5%~8.7%. The linear range of the method was 0.05~0.50 mg/L with the correlation coefficient above 0.99, and the limit of detection and the limits of quantification were 0.001 mg/kg and 0.01 mg/kg, respectively. Conclusion The established method can satisfy the detection requirements of the residue of cyhalothrin in leek. |
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