[多塞过滤净化法联合气相色谱-串联质谱法快速筛选茶叶代用品中125种农药残留]。

Quan Zhang, Yu-Tian Wu, Lei Peng, Shan Bi, Yi-Bing Zhou, Ye Lin, Li-Ya Liu, Qing-Yuan Chen, Xue Zhou
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引用次数: 0

摘要

采用气相色谱-串联质谱(GC-MS/MS)联用快速筛选技术,建立了茶叶代用品基质中125种不同极性农药残留的快速筛选方法。在DB-1701MS石英毛细管柱(30 m×0.25 mm×0.25 μm)上程控温升分离,采用多反应监测(MRM)模式GC-MS/MS检测,基质匹配溶液内标法定量。采用气相色谱-质谱联用法对茶叶代用品中125种代表性农药进行了方法学验证。结果表明,用乙腈水溶液提取茶叶样品的效率最高。M-PFC TD-1色谱柱对铁皮石斛花提取物的纯化效果好,回收率高。优化分析结果表明,125种成分在0.01 mg/L ~ 1.0 mg/L范围内具有良好的线性相关性(R2>0.980)。lod和loq分别为0.003 ~ 0.02 mg/kg (S/N=3)和0.01 ~ 0.05 mg/kg (S/N=10)。125个样品在3个水平上的加样回收率在62.6% ~ 107.6%之间,相对标准偏差(rsd, n=6)为1.0% ~ 13.8%。与其他经典前处理方法相比,该方法不需要活化、平衡、洗脱等步骤,溶剂消耗少,M-PFC TD-1柱纯化效果更好,可直接吸附代茶基质中色素、生物碱等大分子干扰物,操作简便、快速、灵敏度高,适用于散装代茶中农药多组分残留的快速筛选。采用本研究建立的方法对贵州省试点生产企业提供的50份茶代用品样品进行监测,其中2份茶代用品样品中至少检出1种农药残留,检出率为4%。本研究旨在通过了解代茶产品中农药残留的种类和水平,提高制定地方标准指标或技术要求的科学性和实践性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
[Rapid screening of 125 pesticide residues in tea substitutes by multi-plug filtration cleanup method combined with gas chromatography-tandem mass spectrometry].

A rapid screening method for 125 pesticide residues of different polarities in tea substitutes matrix was developed using rapid screening combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). The targets were separated on DB-1701MS quartz capillary column (30 m×0.25 mm×0.25 μm) with programmed temperature rise, detected by GC-MS/MS in multiple reaction monitoring (MRM) mode, and quantified by matrix-matched solution internal standard method. The methodological validation of 125 representative pesticides in tea substitutes was carried out by GC-MS/MS method. The results showed that the tea samples could be extracted most efficiently when using acetonitrile without immersion in water. The M-PFC TD-1 column had a good purification effect on the Dendrobium officinale flower extract with a guaranteed high recovery. The results of optimized analysis showed that the 125 components had a good linear correlation in the range of 0.01 mg/L to 1.0 mg/L (R2>0.980). The LODs and LOQs were 0.003-0.02 mg/kg (S/N=3) and 0.01-0.05 mg/kg (S/N=10),respectively. The recoveries of the 125 targets at three levels were in the range of 62.6%-107.6% with relative standard deviations (RSDs, n=6 of 1.0%-13.8%. Compared with other classical pretreatment methods, this method does not require activation, equilibration and elution steps, consumes less solvent, and the M-PFC TD-1 column shows better purification effect, which can directly adsorb large molecular interferences, such as pigments and alkaloids, in the matrix of the substitute tea, and is easy to operate, rapid, and with high sensitivity, which is suitable for the rapid screening of pesticide multicomponent residues in the bulk substitute tea. The method established in this study was used to monitor 50 samples of tea substitutes provided by the pilot production enterprises in Guizhou Province, in which at least one pesticide residue was detected in two samples of tea substitutes, with a detection rate of 4%. This study aims to enhance the scientific and practical aspects of setting local standard indicators or technical requirements by understanding the types and levels of pesticide residues in substitute tea products.

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