Ingredient Quality Department, The Coca-Cola Company, 1 Coca-Cola Plaza, Atlanta, Georgia 30313, United States.
J Agric Food Chem. 2010 Nov 24;58(22):11553-60. doi: 10.1021/jf102476m. Epub 2010 Oct 20.
This study presents new sample preparation and analytical procedures for the quantification of pesticides on processed tea leaves. The new method includes tea extraction and dispersive solid phase extraction (d-SPE) to prepare gas chromatography (GC) and ultrahigh-performance liquid chromatography (UHPLC)-ready samples, providing a fast and cost-effective solution for time-sensitive industrial analysis to fulfill regulatory requirements. Both GC-negative chemical ionization mass spectrometry (GC-NCI-MS) and UHPLC-tandem mass spectrometry (UHPLC-MS/MS) were employed to produce highly sensitive and reproducible data. Excellent limits of detection (typically below 1 μg/kg for GC and 10 μg/kg for UHPLC), wide linearity ranges, and good recoveries (mostly >70%) were achieved on the selected pesticides. Twenty-seven tea samples purchased from local grocery stores were analyzed using the newly developed methods. Among the pesticides analyzed, endosulfan sulfate and kelthane were the most frequently detected by GC-NCI-MS and imidacloprid and acetamiprid by UHPLC-MS/MS in these teas. The samples were found to be relatively clean, with <1 mg/kg of total pesticide residues. The organic-labeled teas were significantly cleaner than nonorganic ones. The cost per gram of tea did not correlate with pesticide residue levels detected.
本研究提出了新的样品前处理和分析方法,用于定量测定加工茶叶中的农药。新方法包括茶叶提取和分散固相萃取(d-SPE),以制备气相色谱(GC)和超高效液相色谱(UHPLC)就绪样品,为满足监管要求的时间敏感型工业分析提供了快速且具有成本效益的解决方案。GC-负化学电离质谱(GC-NCI-MS)和 UHPLC-串联质谱(UHPLC-MS/MS)均用于生成高灵敏度和重现性数据。在所选择的农药上,均实现了出色的检测限(GC 通常低于 1 μg/kg,UHPLC 通常低于 10 μg/kg)、宽线性范围和良好的回收率(大多数>70%)。使用新开发的方法分析了从当地杂货店购买的 27 个茶叶样品。在所分析的农药中,GC-NCI-MS 最常检测到硫丹硫酸盐和克螨特,而 UHPLC-MS/MS 最常检测到吡虫啉和噻虫胺。这些茶叶中,总农药残留量<1mg/kg,相对较干净。有机标签茶叶比非有机茶叶明显更干净。每克茶叶的成本与检测到的农药残留水平无关。