| 多壁碳纳米管固相萃取气相色谱-串联质谱法测定乌龙茶及土壤中10种三嗪类除草剂残留 |
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投稿时间：2017-05-23
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| 引用本文：方灵,苏德森,刘文静,等.多壁碳纳米管固相萃取气相色谱-串联质谱法测定乌龙茶及土壤中10种三嗪类除草剂残留[J].农药学学报,2017,19(5):617-623. |
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| 基金项目:福建省属公益类科研院所基本科研专项（2016R1024-5）；国家农产品质量安全风险评估专项（GJFP2017005） |
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| 中文摘要:建立了乌龙茶及土壤中10种三嗪类除草剂(西玛津、莠去津、扑灭津、特丁津、敌草净、环丙津、西草净、莠灭净、扑草净和特丁净)残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品经乙腈提取后，以多壁碳纳米管(MWCNTs)、N-丙基乙二胺(PSA)、C18、MgSO4为净化剂分散净化后，在GC-MS/MS多反应监测(MRM)模式下进行测定，空白基质匹配标准曲线外标法定量。研究了不同提取溶剂、不同吸附剂种类及用量对提取净化效率的影响。结果表明：在各自质量浓度范围内(西草净和扑草净在10~500 μg/kg，其余8种除草剂在5~500 μg/kg)具有良好线性关系，相关系数(r)均大于0.99，10种三嗪类除草剂的定量限(LOQ)为5.0~10 μg/kg。在5~100 μg/kg添加水平下，10种三嗪类除草剂在乌龙茶和土壤中的平均回收率在75%~111%之间，相对标准偏差(RSD)在3.1%~8.7%(n=6)之间。该方法操作简单、净化效果好、灵敏度高，具有良好的适用性，能够满足乌龙茶及土壤中10种三嗪类除草剂残留分析测定的要求。 |
| 中文关键词:多壁碳纳米管 气相色谱-串联质谱 乌龙茶 土壤 三嗪类除草剂 残留 |
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| Determination of 10 triazine herbicides residues in oolong tea and soil by gas chromatography-tandem mass spectrometry with multi-walled carbon nanotubes based on solid-phase extraction |
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| Abstract:A gas chromatography-tandem mass spectrometry (GC-MS/MS) method has been developed for detecting 10 triazine herbicides (simazine, atrazine, propazine, terbuthylazine, desmetryn, cyprazine, simetryn, ametryn, prometryn, terbutryn) residues in oolong tea and soil. After extracted by acetonitrile, the samples were purified with multi-walled carbon nanotubes, PSA, C18, MgSO4 and analyzed by GC-MS/MS in multiple reaction monitoring mode. Pesticides were quantified by using the blank matrix matching solution of external standard method. Effects of the type of extraction solvents, and the type and the dosage of adsorbents were then investigated. The results showed that linearity of the curves for 10 triazine herbicides all had correlation coefficients greater than 0.99 (10-500 μg/kg for simetryn and prometryn,5-500 μg/kg for others). The limits of quantifications were 5.0-10 μg/kg. The average recoveries were 75%-111%, and the RSD (n=6) were 3.1%-8.7%. This work provided a method with good applicability, better purifying effect and high sensitivity, which could meet the requirements of triazine herbicides residue analysis in oolong tea and soil. |
| Key words:multi-walled carbon nanotubes GC-MS/MS oolong tea soil triazine herbicides residues |
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