State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(4):713-21. doi: 10.1080/19440049.2013.768777. Epub 2013 Feb 14.
A QuEChERS procedure for the simultaneous determination of pyrimethanil, cyprodinil, mepanipyrim and its metabolite (M31) in fresh and processed fruit and vegetables was developed using ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS). The determination of the four target compounds was achieved in less than 6.0 min using an electrospray ionisation source in positive mode. The limits of detection (LODs) were below 0.4 μg kg⁻¹, while the limits of quantification (LOQs) did not exceed 1.5 μg kg⁻¹ for all studied matrices. Good linearity of the calibration curves was obtained over the range from 0.002 to 2 mg kg⁻¹, with correlation coefficients higher than 0.999. The average recoveries of this method in apple, peach, cabbage and tomato at the five spiked levels (0.002, 0.01, 0.05, 0.20 and 2.0 mg kg⁻¹) ranged from 81.5% to 107.3% with relative standard deviations (RSDs) in the range of 1.5-13.9% (n = 5) for all analytes. Residue levels of anilinopyrimidine fungicides in fresh and home-processed apple, peach, cabbage and tomato were also studied. The results indicate that residue levels are significantly reduced following washing, peeling and boiling, and there is no toxic metabolite of mepanipyrim (M31) which is detected during boiling. This study provides a theoretical basis for China to draw up maximum residue limits (MRLs) and protect consumers from the negative health effects of pesticide residues detected in fruit and vegetables.
建立了超高效液相色谱/串联质谱法(UPLC-MS/MS)测定新鲜和加工果蔬中嘧啶苯胺、环丙嘧啶、甲萘威及其代谢物(M31)的 QuEChERS 方法。在正离子模式下,用电喷雾离子源在 6.0 分钟内即可完成四种目标化合物的测定。四种研究基质的检测限(LOD)均低于 0.4 μg·kg⁻¹,定量限(LOQ)均不超过 1.5 μg·kg⁻¹。校准曲线在 0.002-2 mg·kg⁻¹范围内具有良好的线性关系,相关系数均高于 0.999。该方法在苹果、桃、白菜和番茄五种加标水平(0.002、0.01、0.05、0.20 和 2.0 mg·kg⁻¹)的平均回收率为 81.5%-107.3%,相对标准偏差(RSD)在 1.5%-13.9%(n = 5)之间。还研究了新鲜和家庭加工苹果、桃、白菜和番茄中苯胺嘧啶类杀菌剂的残留水平。结果表明,清洗、去皮和煮沸后残留水平显著降低,煮沸过程中未检测到甲萘威(M31)的有毒代谢物。本研究为中国制定最大残留限量(MRL)提供了理论依据,以保护消费者免受果蔬中农药残留带来的健康负面影响。