QuEChERS-三重四极杆气质联用法测定大米中12种农药残留量
目的 建立一种采用QuEChERS前处理技术结合三重四极杆气质联用法(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)同时测定大米中12种农药残留量的检测方法。方法 样品经乙腈提取、采用无水硫酸镁、C18、乙二胺-N-丙基硅烷(primary secondary amine, PSA)作为吸附剂, 净化提取液, 浓缩过滤后的样品用气相色谱质谱联用仪进行检测。结果 12种农药在0.004~0.40 μg/mL范围内线性关系良好, 相关系数均大于0.997。在0.04、0.08、0.12 mg/kg 3个加标水平下, 12种农药的平均回收率为81.08%~114.50%, 精密度为0.48%~4.92%(n=6), 最低检出限为0.01 mg/kg。结论 该方法样品处理简便、快捷、高效、重复性和稳定性良好, 可用于大米中12种农药的定量检测与定性认证。
Objective To establish a method for the simultaneous determination of 12 kinds of pesticide residues in rice by QuEChERS-gas chromatography-triple quadrupole mass spectrometry. Methods Samples were extracted by acetonitrile, the extract was purified using anhydrous magnesium sulfate, C18, PSA as adsorbent, and the concentrated and filtered samples were tested by gas chromatography-triple quadrupole mass spectrometry. Results The 12 kinds of pesticides had good linear relationship in the range of 0.004-0.40 μg/mL, and the correlation coefficient was greater than 0.997. The recoveries at 3 spiked levels of 0.04、0.08、0.12 mg/kg of 12 pesticides ranged from 81.08% to 114.50%, with the precision from 0.48 to 4.92% (n=6). The limit of detection was 0.01 mg/kg. Conclusion This method is easy, simple, fast, efficient, good repeatability and stability, which can be used for the quantitative detection and qualitative identification of 12 kinds of pesticides in rice.
标题：QuEChERS-三重四极杆气质联用法测定大米中12种农药残留量
英文标题：Determination of 12 kinds of pesticide residues in rice by QuEChERS-gas chromatography-triple quadrupole mass spectrometry
作者：
乔海霞 山东标准检测技术有限公司
曹宁 中华全国供销合作总社济南果品研究院
蔡可文 山东标准检测技术有限公司
刘建洋 山东标准检测技术有限公司
中文关键词:大米,QuEChERS,三重四极杆气质联用法,农药残留,
英文关键词:rice,QuEChERS,gas chromatography-triple quadrupole mass spectrometry,pesticide residues,
发表日期：2019-04-01
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