Study On Detection Methods Of Triazole Fungicides In Chrysanthemum,Fritillaries And Animal-Derived Foods

As the largest and most diverse class of fungicides,triazole fungicides are commonly used for pest control.Advanced countries such as Japan's“positive list system”,the International Codex Alimentarius Commission?CAC?standards have established strict residue limits for some triazole fungicides.However,the residue limit standards for triazole fungicides in China are not perfect,and there are problems involving single parameters of triazoles and fewer types of foods.With the development of the economy,people pay more attention to food safety.Therefore,this paper establishes the analysis and detection methods of triazole fungicides in different complex matrices by optimizing pre-treatment conditions and instrument conditions.The specific contents are as follows:1.A selective accelerated solvent extraction method combined with UPLC-MS/MS was used to determine the triazole fungicides in Chrysanthemum morifolium and Fritillaria.The method completed the extraction and purification in the same step,which simplified the experimental step.The acetonitrile was used as the extraction solvent at 90°C and the mixed adsorbent(PSA+C₁₈+GCB)as the purification materials.The recoveries of the analytes were ranged from 70.2%to 96.9%.At three adding levels?10,50 and 100?g/kg?,while the LODs and the LOQs were 0.6-3.0?g/kg and 2.1-10.0?g/kg respectively.The results indicated this method is a simple,rapid and sensitivity method for the analysis of triazole fungicides in Chrysanthemum morifolium and Fritillaria which can meet the requirements of daily inspection.2.A method for the determination of triazole fungicide residues in animal tissue samples by the through type solid phase extraction combined with UPLC-MS/MS was developed and validated.The pork,pig liver and its fat samples were extracted by acetonitrile.The concentrated extract mixed with water then passed through a PRiME HLB column without activation and equilibrium.The effluent was directly determined by UPLC-MS/MS.During the purification process,the impurities such as fats and phospholipids were retained on the column which could minimize matrix interferences and enhance the experimental efficiency.With the optimal conditions,there coveries of those triazole fungicides ranged from 69.5%to 109.5%at the three spiking levels examined?2?g/kg,5?g/kg and 10?g/kg?and the relative standard deviation ranged from 0.4%to 10.8%.The LODs and LOQs were between 0.3-0.6?g/kg and 1.0-2.0?g/kg respectively.The method could remove the impurities in larger extent,which can be applied to detect triazole fungicides in liver,fat and muscle tissues of livestock and poultry products.3.A method was developed for the determination of triazole fungicide residues in poultry eggs and liquid milk by high-efficiency purification with UPLC-MS/MS.The sample was extracted with acetonitrile,salted out and dehydrated,concentrated,and purified by PRiME HLB solid phase extraction column.At three adding levels?2?g/kg,5?g/kg,and 10?g/kg?,the recovery rates of 21triazole fungicides were ranged from 70.3%to 99.3%,and the relative standard deviation was2.1%-11.0%.The LODs and LOQs were 0.2-0.6?g/kg and 0.5-2.0?g/kg respectively.The method is sensitivity and stable which can be used in the determination the quantitation of various triazole fungicides in eggs and liquid milk.