艾小勇 1, 2 , 任志芹 1, 3 , 袁 飞 1 , 原保忠 2 , 张 元 1 , 李伟青 1 , 张 峰 1.改进的 QuEChERS -气相色谱-串联质谱法
测定鲜烟叶中 27 种农药残留[J].广东农业科学,2015,42(17):96-101 |
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改进的 QuEChERS -气相色谱-串联质谱法
测定鲜烟叶中 27 种农药残留 |
Determination of 27 pesticide residues in fresh tobaccoleaves with modified-QuEChERS by gaschromatography-tandem mass spectrometry |
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DOI: |
中文关键词: QuEChERS 复合吸附剂 农药残留 鲜烟叶 气相色谱-串联质谱 |
英文关键词: QuEChERS compound adsorbent pesticide residues fresh tobacco leaves gas chromatography-
tandem mass spectrometry(GC-MS/MS) |
基金项目:国家重大仪器设备开发专项(2012YQ
14000806);国家质检总局质检公益性行业科研专项
(201310134, 201410088-02) ; 国家质检总局科技计划项
目(2013IK202) |
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中文摘要: |
建立了鲜烟叶中 27 种农药的气相色谱 -串联质谱(GC-MS/MS)检测方法。 样品以乙腈为提
取溶剂, 对鲜烟叶中 27 种农药进行提取, 采用 N-丙基乙二胺(PSA) 、 C 18 和石墨化碳黑(GCB)3 种复合
吸附剂净化, 采用 GC-MS/MS 在多反应监测(MRM)模式下进行检测, 基质匹配外标法定量。 结果显示,
27 种农药在 10~1 000 μg/kg 范围内, 线性相关系数(r 2 )均大于 0.995, 检出限(LOD)为 0.4~2.9 μg/kg,
定量限(LOQ)为 1.4~9.6 μg/kg, 在 3 个添加水平下的回收率为 71.8%~108.1%, 相对标准偏差(RSD)为
3.2%~11.8%。 该方法前处理简单快速, 准确度和精密度均符合农药多残留检测技术的要求, 适用于鲜烟叶中
27 种农药残留的快速筛查和测定。 |
英文摘要: |
A GC-MS/MS method was established for simultaneous determination of 27 pesticides in fresh tobacco
leaves. Using acetonitrile as extraction solvent and including a cleanup step with primary secondary amine(PSA) ,
graphitized carbon black(GCB)and C 18 to reduce the high matrix effect found in these products. The samples were
quantified using external standard with the matrix matched standard calibration curve method. Good linearities of two
suckercides were observed in the range of 10-1 000 µg/kg with correlation coefficients more than 0.995. The limits
of detection(LOD)and the limits of quantification(LOQ)for 27 pesticides were 0.4-2.9 μg/kg and 1.4-9.6
μg/kg, respectively. The average recoveries at three spiked concentration levels ranged from 71.8% to 108.1%. The
repeatabilities expressed as relative standard deviations(RSD)ranged from 3.2% to 11.8%. The method was suitable
for the determination of 27 pesticide residues in fresh tobacco leaves. |
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