Taylor Michael J, Keenan George A, Reid Kirsty B, Fernández Diana Uría
The Scottish Government, SASA, Roddinglaw Road, Edinburgh EH12 9FJ, UK.
Rapid Commun Mass Spectrom. 2008 Sep;22(17):2731-46. doi: 10.1002/rcm.3671.
The utility of ultra-performance liquid chromatography/orthogonal-acceleration time-of flight mass spectrometry (UPLC/TOFMS) for the rapid qualitative and quantitative analysis of 100 pesticides targeted in strawberry was assessed by comparing results with those obtained using a validated in-house UPLC tandem mass spectrometry (MS/MS) multi-residue method. Crude extracts from retail strawberry samples received as part of the 2007 annual UK pesticide residues in food surveillance programme were screened for the presence of pesticide residues using UPLC/TOFMS. Accurate mass measurement of positive and negative ions allowed their extraction following 'full mass range data acquisition' with negligible interference from background or co-eluting species observed during UPLC gradient separation (in a cycle time of just 6.5 min per run). Extracted ion data was used to construct calibration curves and to detect and identify any incurred residues (i.e. pesticides incorporated in or on the test material following application during cultivation, harvest and storage). Calibration using matrix-matched standards was performed over a narrow concentration range of 0.005-0.04 mg kg(-1) with determination coefficients (r2) > or =0.99 for all analytes with the exception of malathion/fenarimol/fludioxanil (r2 = 0.98), quassia/pymetrazine (r2 = 0.97) and fenthion sulfone (r2 = 0.95). Residues found in selected samples ranged from 0.025-0.28 mg kg(-1) and were in excellent agreement with results obtained using UPLC/MS/MS. Mass measurement accuracies of < or =5 ppm were achieved consistently throughout the separation, mass range and concentration range of interest thus providing the opportunity to obtain discrete elemental compositions of target ions.
通过将超高效液相色谱/正交加速飞行时间质谱法(UPLC/TOFMS)的结果与使用经过验证的内部超高效液相色谱串联质谱法(MS/MS)多残留方法获得的结果进行比较,评估了该方法对草莓中100种目标农药进行快速定性和定量分析的实用性。作为2007年英国食品农药残留年度监测计划一部分收到的零售草莓样品的粗提物,使用UPLC/TOFMS筛选农药残留的存在情况。在“全质量范围数据采集”后,通过对正离子和负离子进行精确质量测量来提取它们,在UPLC梯度分离过程中(每次运行的循环时间仅为6.5分钟),背景或共洗脱物质的干扰可忽略不计。提取的离子数据用于构建校准曲线,并检测和识别任何残留的农药(即在种植、收获和储存过程中施用于测试材料中或其上的农药)。使用基质匹配标准品在0.005 - 0.04 mg kg⁻¹的窄浓度范围内进行校准,除马拉硫磷/氯苯嘧啶醇/咯菌腈(r² = 0.98)、苦木素/嘧菌胺(r² = 0.97)和倍硫磷砜(r² = 0.95)外,所有分析物的测定系数(r²)≥0.99。选定样品中发现的残留量范围为0.025 - 0.28 mg kg⁻¹,与使用UPLC/MS/MS获得的结果高度一致。在整个感兴趣的分离、质量范围和浓度范围内,始终实现了≤5 ppm的质量测量精度,从而为获得目标离子的离散元素组成提供了机会。