Detection Of Pesticide Residues In Honeysuckle And Chrysanthemum Using Modified QuEChERS Method With Chromatography-Tandem Mass Spectrometry

The application of Chinese herbal medicine has been in China for thousands of years.Honeysuckle and chrysanthemum are used as two kinds of commonly used Chinese herbal medicines.With the continuous development of Chinese medicine,the demand is increasing and the planting area is expanding.However,these two herbs are susceptible to pest and disease damage during planting,and growers often use pesticides to ensure their yield.The problem of pesticide residues in honeysuckle and chrysanthemum has only attracted attention from all parties in recent years.The relevant pesticide residue limit standards are few,which will affect the import and export trade of honeysuckle and chrysanthemum in China to a certain extent,and slow down the modernization and internationalization of Chinese herbal medicine industry.pace of.Therefore,it is necessary to develop a fast and accurate detection method.In this paper,the improved QuEChERS technique was combined with gas chromatography-tandem mass spectrometry and ultra performance liquid chromatography-tandem mass spectrometry to analyze 134 pesticides in honeysuckle and chrysanthemum.The results were mainly satisfactory.The specific results and conclusions are as follows:1.The traditional QuEChERS technology was improved,and combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and gas chromatography tandem mass spectrometry(GC-MS/MS)to determine 134 pesticide residues in chrysanthemum and honeysuckle.The sample was extracted with 0.1% acetic acid in acetonitrile,and the magnetic nanomaterial was adsorbed by an external magnetic field to promote delamination instead of the conventional centrifugation step,and the complex substrate Sin-QuEChERS Nano purification column was used for purification.The purification effect is improved,which saves time and reduces the loss of target caused by solution transfer.2.The detection method established in the experiment was verified by two methods: honeysuckle and chrysanthemum.The detection limit(LOD)of honeysuckle was between 0.12?g/kg and 3.00?g/kg,and the limit of quantification(LOQ)was 0.40?g/kg.~10.00?g/kg;the detection limit(LOD)of chrysanthemum was between 0.11?g/kg~2.84?g/kg?g/kg,and the limit of quantitation(LOQ)was between 0.37?g/kg~9.47?g/kg.The linear correlation coefficient R2 ? 0.990,the linear relationship is good;the addition recovery experiment and precision test are carried out in two matrices.The average recoveries of honeysuckle and chrysanthemum at 10?g/kg,50?g/kg and 100?g/kg ranged from 70.33% to 119.56% and 71.10% to 114.53%,respectively.The relative standard deviation(RSD)ranged from 0.14% to 14.68.Between 1.00 and 14.47%.3.Collecting honeysuckle and chrysanthemums from various districts and counties in Tai'an City,and the national standard "GB 23200.10-2016 Determination of 488 pesticides and related chemical residues in mulberry branches,honeysuckle,medlar and lotus leaves by gas chromatography-mass spectrometry" "GB 23200.11-2016 mulberry,honeysuckle,hazelnut and lotus leaf determination of 413 pesticides and related chemical residues determination liquid chromatography-mass spectrometry" method comparison,the detection results of the two methods are basically the same.4.134 kinds of pesticide residues were detected in 266 actual samples of the two substrates.The detection rate of positive samples was 42.8%.Seven pesticides were detected,which were common fungicides and insecticides in agricultural production.Some of the honeysuckle samples were imidacloprid.(317.6 ?g/kg)and thiophanate-methyl(463.5 ?g/kg)detected higher residual amounts.