Christensen H B, Granby K
Danish Veterinary and Food Administration, Søborg.
Food Addit Contam. 2001 Oct;18(10):866-74. doi: 10.1080/02652030121435.
Strobilurins are a new class of fungicides that are active against a broad spectrum of fungi. In the present work a GC method for analysis of strobilurin fungicides was validated. The method was based on, extraction with ethyl acetate/cyclohexane, clean-up by gel permeation chromatography, (GPC) and determination of the content by gas chromatography (GC) with electron capture (EC-), nitrogen/phosphorous (NP-), and mass spectrometric (MS-) detection. Three strobilurins, azoxystrobin, kresoxim-methyl and trifloxystrobin were validated on three matrices, wheat, apple and grapes. The validation was based on recovery tests at three or four spiking levels, determined as double determinations and repeated three times (n = 6). The mean recoveries for the three detectors were in the range of 70-114%, and the LODs were between 0.004 mg/kg and 0.014 mg/kg, for all three strobilurins. The values for repeatability and reproducibility were within the limits for repeatability and reproducibility given by the Horwitz equation. Validation was not accepted for azoxystrobin in grapes on all three detectors and for azoxystrobin in apple for the MS-detector. A comparison of matrix-matched standards versus standards in solvent showed varying differences between the two calibration curves.
甲氧基丙烯酸酯类杀菌剂是一类新型杀菌剂，对多种真菌具有活性。在本研究中，一种用于分析甲氧基丙烯酸酯类杀菌剂的气相色谱方法得到了验证。该方法基于用乙酸乙酯/环己烷萃取、通过凝胶渗透色谱（GPC）净化以及用带电子捕获（EC-）、氮/磷（NP-）和质谱（MS-）检测的气相色谱（GC）测定含量。三种甲氧基丙烯酸酯类杀菌剂，即嘧菌酯、醚菌酯和肟菌酯，在小麦、苹果和葡萄三种基质上进行了验证。验证基于在三个或四个加标水平下的回收率测试，以双份测定确定并重复三次（n = 6）。对于所有三种甲氧基丙烯酸酯类杀菌剂，三种检测器的平均回收率在70 - 114%范围内，检测限在0.004 mg/kg至0.014 mg/kg之间。重复性和再现性的值在Horwitz方程给出的重复性和再现性限度内。对于葡萄中的嘧菌酯在所有三种检测器上以及苹果中的嘧菌酯在MS检测器上，验证未被接受。基质匹配标准品与溶剂中的标准品的比较显示两条校准曲线之间存在不同差异。
