中文摘要：本文以果蔬农残为检测样本进行气相色谱-电子电离-全扫描高分辨率-质谱法的应用评估。经过详细的评估和讨论发现，该方法最佳检测条件为在全扫描模式（m/z 50-500）下分辨率是60,000，自动增益控制目标值为3×106。在此条件下：（1）在较大的浓度范围下，最佳质谱精度可达到2 ppm以内；（2）扫面速度最小达到12S/P；（3）内部扫描动力范围较广，足以检测到果蔬基质中大多数浓度在0.5pg的农药残留。本文还对三种基质（西红柿、韭菜和橘子）中10μg/kg和50μg/kg 的54种农药残留量进行定量检测分析实证。结果显示，大多数农药残留的回收率在70-120%之间，可重复性标准差小于10%。气相色谱-电子电离-全扫描高分辨率-质谱法可广泛适用于农药残留检测，定性地扩大范围筛选潜力使得其具有较大的优势替代气相色谱-三重四极杆质谱法。
外文摘要：Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50-500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of +/- 5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs <= 0.5 pg in fruit/vegetable matrices (corresponding to <= 0.5 mu g kg(-1)) for most pesticides. EI-Orbitrap spectra were consistent over a very wide concentration range (5 orders) with good match values against NIST (EI-quadrupole) spectra. The applicability for quantitative residue analysis was verified by validation of 54 pesticides in three matrices (tomato, leek, orange) at 10 and 50 mu g/kg. The method involved a QuEChERS-based extraction with a solvent switch into iso-octane, and 1 mu L hot splitless injection into the GC-HRMS system. A recovery between 70 and 120% and a repeatability RSD <10% was obtained in most cases. Linearity was demonstrated for the range <= 5-250 mu g kg(-1). The pesticides could be identified according to the applicable EU criteria for GC-HRMS (SANTE/11945/2015). GC-EI-full scan Orbitrap HRMS was found to be highly suited for quantitative pesticide residue analysis. The potential of qualitative screening to extend the scope makes it an attractive alternative to GC-triple quadrupole MS.
外文关键词：Gas chromatography, High resolution mass spectrometry, Electron ionization, Orbitrap, Pesticide residue analysis, Food
作者：Mol, Hans G. J.; Tienstra, Marc; Zomer, Paul
作者单位：RIKILT Wageningen UR, Akkermaalsbos 2, NL-6708 WB Wageningen, Netherlands.
期刊名称：ANALYTICA CHIMICA ACTA
期刊影响因子：4.712
出版年份：2016
出版刊次：9
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