Determination of 32 Fungicide Residues in Tea by Gas Chromatography-Tandem Mass Spectrometry
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摘要: 建立了茶叶中32种杀菌剂类农药残留的气相色谱-串联质谱（GC-MS/MS）测定方法。样品经乙腈高速匀浆提取后，以N-丙基乙二胺（PSA）、石墨化碳（GCB）、C18为净化剂进行净化，在GC-MS/MS多反应离子监测（MRM）模式下进行测定，空白基质匹配标准曲线外标法定量。结果表明：27种杀菌剂在10~1 000 μg·L-1，5种杀菌剂在20~1 000 μg·L-1范围内具有良好线性关系，相关系数（R2）均大于0.99。方法检出限（S/N≥3）为0.1~8.1 μg·L-1，定量限（S/N≥10）为0.4~23.4 μg·L-1，平均添加回收率范围为70.4%~109.1%，相对标准偏差（RSD）3.4%~10.3%。该方法样品前处理操作简单、净化效果好、灵敏度高，具有良好的适用性，能够满足茶叶中多种杀菌剂残留测定分析的要求。Abstract: A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for detecting 32 fungicide residues in teas.The samples were extracted by acetonitrile under high-speed homogenization, purified with PSA, GCB, C18, and determined by GC-MS/MS in multi-reaction ion monitoring mode. Pesticide contents were determined by using the standard curves constructed with solutions of respective external standards. Linearity of the curves for 27 pesticides ranged from 10 μg·L-1 to 1 000 μg·L-1, and from 20 μg·L-1 to 1 000 μg·L-1 for the remaining 5 pesticides, with correlation coefficients greater than 0.99. The limits of detection were 0.1-8.1 μg·L-1 (S/N ≥ 3); and, those of quantification, 0.4-23.4 μg·L-1 (S/N ≥ 10). The average recovery rates were 70.4%-109.1%; and RSD (n=6) 3.4%-10.3%. The newly developed highly sensitive methodology that required simple pre-treatment and effective purification procedures appeared to be appropriate for the detection of fungicide residues in teas.
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Key words:
- fungicides /
- tea /
- GC-MS/MS
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图 1 32种杀菌剂(分为2组)混合标准溶液的总离子流色谱
Figure 1. TIC chromatogram of 32 pesticides in two groups
表 1 32种杀菌剂质谱信息
Table 1. Information on mass spectrum for 32 pesticides
表 2 不同提取溶剂对茶叶中32种杀菌剂的添加回收率
Table 2. Recovery rates on spiked 32 pesticides extracted with various solvents from tea
表 3 32种农药回收率及其检出限(LOD)、定量限(LOQ)、相对标准偏差(RSD)(n=6)
Table 3. Recoveries, limits of detection (LOD), limits of quantification (LOQ), and relative standard deviations (RSD) of 32 pesticides (n=6)
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