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首页> 美国卫生研究院文献>Springer Open Choice >Qualitative aspects and validation of a screening method for pesticides in vegetables and fruits based on liquid chromatography coupled to full scan high resolution (Orbitrap) mass spectrometry
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Qualitative aspects and validation of a screening method for pesticides in vegetables and fruits based on liquid chromatography coupled to full scan high resolution (Orbitrap) mass spectrometry

机译：基于液相色谱-全扫描高分辨率（Orbitrap）质谱联用的蔬菜和水果中农药筛查方法的定性和验证

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The analytical capabilities of liquid chromatography with single-stage high-resolution mass spectrometry have been investigated with emphasis on qualitative aspects related to selective detection during screening and to identification. The study involved 21 different vegetable and fruit commodities, a screening database of 556 pesticides for evaluation of false positives, and a test set of 130 pesticides spiked to the commodities at 0.01, 0.05, and 0.20 mg/kg for evaluation of false negatives. The final method involved a QuEChERS-based sample preparation (without dSPE clean up) and full scan acquisition using alternating scan events without/with fragmentation, at a resolving power of 50,000. Analyte detection was based on extraction of the exact mass (±5 ppm) of the major adduct ion at the database retention time ±30 s and the presence of a second diagnostic ion. Various options for the additional ion were investigated and compared (other adduct ions, M + 1 or M + 2 isotopes, fragments). The two-ion approach for selective detection of the pesticides in the full scan data was compared with two alternative approaches based on response thresholds. Using the two-ion approach, the number of false positives out of 11,676 pesticide/commodity combinations targeted was 36 (0.3 %). The percentage of false negatives, assessed for 2,730 pesticide/commodity combinations, was 13 %, 3 %, and 1 % at the 0.01-, 0.05-, and 0.20-mg/kg level, respectively (slightly higher with fully automated detection). Following the SANCO/12495/2011 protocol for validation of screening methods, the screening detection limit was determined for 130 pesticides and found to be 0.01, 0.05, and ≥0.20 mg/kg for 86, 30, and 14 pesticides, respectively. For the detected pesticides in the spiked samples, the ability for unambiguous identification according to EU criteria was evaluated. A proposal for adaption of the criteria was made.>FigureExtracted ion chromatograms showing availability of various diagnostic ions after analysis by LC with full scan high resolution MS, enabling selective detection nd identification of pesticides. Example shown: propoxur at 0.01 mg/kg in apple.
机译：已经研究了具有单级高分辨率质谱的液相色谱的分析能力，重点是与筛选和鉴定过程中选择性检测有关的定性方面。该研究涉及21种不同的蔬菜和水果商品，用于评估假阳性的556种农药的筛查数据库以及以0.01、0.05和0.20 mg / kg的含量加到商品中的130种农药的测试集以用于评估假阴性。最终方法涉及基于QuEChERS的样品制备（无需dSPE净化）和使用交替扫描事件（不带碎片或带碎片）的全扫描采集，分辨率为50,000。分析物的检测是基于在数据库保留时间±30 s内提取主要加合离子的精确质量（±5 ppm）和第二诊断离子的存在。对附加离子的各种选择方案进行了研究和比较（其他加合物离子，M +1或M +2同位素，碎片）。基于响应阈值，在全扫描数据中选择性检测农药的双离子方法与两种替代方法进行了比较。使用双离子方法，目标11676种农药/商品组合中的假阳性数为36（0.3％）。在0.01-，0.05-和0.20 mg / kg的水平下，对2,730种农药/商品组合进行评估的假阴性百分比分别为13％，3％和1％（全自动检测时略高）。按照SANCO / 12495/2011协议进行筛查方法的验证，确定了130种农药的筛查检出限，发现86、30和14种农药分别为0.01、0.05和≥0.20mg / kg。对于加标样品中检测到的农药，评估了根据欧盟标准进行明确鉴定的能力。提出了适应标准的建议。<！-fig ft0-> <！-fig @ position =“ anchor” mode = article f4-> <！-fig mode =“ anchored” f5-- > >图<！-fig / graphic | fig / alternatives / graphic mode =“ anchored” m1-> <！-标题a7->提取的离子色谱图，显示了通过LC分析后各种诊断离子的可用性全扫描高分辨率质谱仪，可选择性检测和鉴定农药。显示的示例：苹果中的丙草胺含量为0.01 mg / kg。

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