Wang Jian, Chow Willis, Wong Jon W
Canadian Food Inspection Agency, Calgary Laboratory, 3650-36th Street N.W, Calgary, Alberta, T2L 2L1 Canada.
US Food and Drug Administration, Human Foods Program, 5001 Campus Drive, College Park, Maryland, 20740 USA.
J AOAC Int. 2025 Feb 18. doi: 10.1093/jaoacint/qsaf009.
Cost-effective multi-residue pesticide methods with a broad detection scope are desired for risk-based monitoring programs.
The aim was to evaluate the nDATA (non-target Data Acquisition for Target Analysis) workflow using UHPLC/ESI quadrupole-Orbitrap (Q-Orbitrap) mass spectrometry and semi-quantitate 1094 pesticides in fruits and vegetables.
Pesticide extracts from fresh produce were prepared using the QuEChERS procedure. nDATA was carried out by utilizing UHPLC/ESI Q-Orbitrap Full MS scan and variable data independent acquisition (vDIA). Data were processed using a Compound Database (CDB, 1094 pesticides) and one-point standard calibration with internal standards for semi-quantitation. Data processing criteria were based on retention time (± 0.5 min) and mass accuracy of a precursor ion (± 5 ppm) (RTP by full MS), or retention time (± 0.5 min) and mass accuracy of a precursor ion (± 5 ppm) and that of its fragment ion (± 10 ppm) (RTFI by full MS/vDIA).
RTP found 1010 and 1094 pesticides, while RTFI identified 906 and 1029 pesticides at 10 and 100 μg/kg, respectively. RTF detected all 30 LC-amenable pesticides and RTFI identified 29 of 30 LC-amenable pesticides in eight proficiency testing samples. There were 42 pairs of co-eluting isomeric pesticides and five pairs of isobaric pesticides that were not separated by mass resolving power and/or chromatographic separation (ΔtR < 0.12 min) with the current instrument parameter settings.
The validated nDATA workflow using UHPLC/ESI Q-Orbitrap Full MS/vDIA proved to be a comprehensive detection method for semi-quantitative screening of 1094 pesticides in fruits and vegetables.
nDATA combines both non-target data acquisition and target analysis. The non-target data acquisition generates data for retrospective analysis of a large number (over one thousand) of pesticides. The target analysis using a compound database (CDB) and a one-point standard calibration affords confidence in semi-quantitative screening results.
基于风险的监测项目需要具有广泛检测范围且经济高效的多残留农药检测方法。
旨在评估使用超高效液相色谱/电喷雾四极杆-轨道阱（Q-轨道阱）质谱的nDATA（用于目标分析的非目标数据采集）工作流程，并对水果和蔬菜中的1094种农药进行半定量分析。
采用QuEChERS方法制备新鲜农产品的农药提取物。利用超高效液相色谱/电喷雾Q-轨道阱全扫描和可变数据非依赖采集（vDIA）进行nDATA分析。使用化合物数据库（CDB，1094种农药）和内标单点标准校准对数据进行处理以进行半定量分析。数据处理标准基于保留时间（±0.5分钟）和母离子的质量准确度（±5 ppm）（全扫描的RTP），或保留时间（±0.5分钟）、母离子的质量准确度（±5 ppm）及其碎片离子的质量准确度（±10 ppm）（全扫描/vDIA的RTFI）。
RTP在10和100 μg/kg时分别发现了1010种和1094种农药，而RTFI分别鉴定出906种和1029种农药。在8个能力验证样品中，RTF检测到了所有30种适用于液相色谱分析的农药，RTFI鉴定出了30种适用于液相色谱分析的农药中的29种。在当前仪器参数设置下，有42对共洗脱的同分异构农药和5对同量异位农药未通过质量分辨率和/或色谱分离（ΔtR < 0.12分钟）分开。
经验证的使用超高效液相色谱/电喷雾Q-轨道阱全扫描/vDIA的nDATA工作流程被证明是一种用于水果和蔬菜中1094种农药半定量筛查的综合检测方法。
nDATA结合了非目标数据采集和目标分析。非目标数据采集生成的数据可用于对大量（超过一千种）农药进行回顾性分析。使用化合物数据库（CDB）和单点标准校准的目标分析为半定量筛查结果提供了可信度。
