| The yield and planting area of traditional Chinese medicine are increasing every year,and the problem of pesticide residues in traditional Chinese medicine is also becoming more and more serious.People will take the traditional Chinese medicine decoction made from the pieces by soaking and decoction.Whether the pesticide residues will change during the decoction process of traditional Chinese medicine pieces and whether the decoction is risky to intake are the focus of the research on the quality and safety of traditional Chinese medicine.However,there are few reports on the literature.In this paper,a multi-residues analysis method for 17 fungicides in Paeoniae Radix Alba pieces was established by using QuEChERS method combined with UPLC-MS/MS,and the method has been applied to detect 103 commercial Paeoniae Radix Alba pieces sample collected from 12 provinces and cities nationwide.According to the results of the detection of fungicides in commercial Paeoniae Radix Alba pieces samples,5 fungicides including carbendazim,epoxiconazole,tebuconazole,propiconazole and difenoconazole were selected as research objects,study their residual behavior and processing factors in decoction process of Paeoniae Radix Alba pieces.Based on the detection results and the processing factors,the dietary exposure risks of the 5 tested fungicides residues during the Paeoniae Radix Alba pieces decoction process were evaluated.The research results have theoretical guiding significance and practical application value for scientific evaluation of Paeoniae Radix Alba safety,control of pesticide residue pollution on Paeoniae Radix Alba,risk management and improvement of Paeoniae Radix Alba chalk quality.The main results were as following:1.Residues of fungicides in commercial Paeoniae Radix Alba pieces sampleA multi-residues analysis method for 17 fungicides on Paeoniae Radix Alba pieces was established by using QuEChERS method combined with UPLC-MS/MS.The sensitivity of the method was good,and the correlation coefficients were greater than 0.93.The LOD and LOQ were 0.03-2.14 ?g·kg-1 and 0.10-6.58 ?g·kg-1,respectively.The external standard method and matrix standard method were used to determine the recovery rate of 17 tested fungicides in the Paeoniae Radix Alba pieces,under the spiked levels of 50,100,1000 ?g·kg-1,the average recovery rate of 17 tested fungicides in Radix Paeoniae Alba pieces was between 68.49%and 114.95%,and the relative standard deviation was within the range of 2.17%to 12.42%.The method has good accuracy and precision,and meet the requirements of pesticide residue analysis.17 fungicides residues were detected in 103 samples of Paeoniae Radix Alba pieces collected in 12 provinces and cities nationwide in 2017-2018.And 8 kind of fungicides were detected out.The probability of detecting more than 4 pesticides in a single sample is higher than 99%.The detection rate of carbendazim was the highest,100%,followed by epoxiconazole,99.03%,the detection rate of tebuconazole,difenoconazole and propiconazole was all higher than 37%.The detected concentration of 17 tested fungicides was within the range of 0.14-284.30 ug-kg'1,the average concentration was between 0.34 ug-kg'1 and 15.83 ug-kg"1,the median concentration was between 0.33 ug-kg'1 and 13.88 ug-kg"1.2.LC-MS/MS analysis method of the 5 fungicides residues in the Paeoniae Radix Alba decoctionA multi-residues analysis methods for the 5 fungicides in Paeoniae Radix Alba decoction was established.In the concentration range of 5-1000 ug-kg'1,the sensitivitythe of the method is good,and the correlation coefficient R2 is greater than 0.999.The LOD and LOQ of the 5 tested fungicides were 0.69-2.10 ug-kg-1 and 2.29-7.01 ug-kg-1,respectively.Under the spiked levels of 20,200,1000 ug-kg"1,the average recovery rate of 5 fungicides in Radix Paeoniae Alba decoction was between 82.49%and 104.05%,and the relative standard deviation was within the range of 0.36-5.29%,the method for the 5 fungicides in Paeoniae Radix Alba decoction has good accuracy and precision,and meet the requirements of pesticide residue analysis.3.Residual dynamic of the 5 tested fungicide residues during the decoction process of Paeoniae Radix Alba piecesIn this paper,different time parameters were set for the soaking,first decoction,second decoction and concentration experiments of Paeoniae Radix Alba pieces,which reference the "Research strategies in standard decoction of medicinal slices".During the soaking process,the residues of carbendazim,epoxiconazole,tebuconazole,propiconazole and difenoconazole were mainly transferred from the pieces to the decoction.During the first decoction process,the residues of the 5 tested fungicides in the decoction was increased first and then decreased,peaked at 30 min or 40 min respectively.The residues of the 5 tested fungicides in the pieces decreased with time.In the second decoction process,the residues of the 5 fungicides is basically similar to that of the first decoction.The residues of the 5 tested fungicides in the decoction was increased first and then decreased,peaked at 20 min or 30 min,respectively.The residues of the 5 tested fungicides in the pieces decreased with time.During the concentration process,the residues of the 5 fungicides did not change with the degree of concentration.The residues of the 5 tested fungicides were 76.10,40.50,58.42,55.11 and 56.23 ?g when concentrated to 250 mL.4.Processing factors and dietary exposure risks of the 5 tested fungicide residues during the decoction process of Paeoniae Radix Alba piecesDuring the decoction process of Paeoniae Radix Alba pieces,the processing factors of the carbendazim,flucyclazole,tebuconazole,propiconazole and difenoconazole were 0.3796,0.2876,0.3260,0.2956 and 0.3972,respectively.The residues of the 5 tested fungicides in the Paeoniae Radix Alba decoction made by the standard decoction process was less than 40%in the pieces before the decoction process.The application point evaluation model combined with the processing factors of the 5 tested fungicides residues in the decoction process was used to evaluate the risk of chronic,acute and cumulative dietary intake risk of the 5 tested fungicides residues during the decoction process of Paeoniae Radix Alba pieces.The risk of chronic,acute and cumulative dietary intake of the 5 tested fungicides residues were 4.2234×10-4-3.3262×10-2,5.373l×10-4-0.2570 and 0.0520,respectively,within the acceptable range.The acute risk quotient HQa of carbendazim was higher than the other fungicides,which was 0.2570.Carbendazim,epoxiconazole and Difenoconazole accounted for 14.15%,63.95%and 17.82%of the cumulative risk CI,respectively. |
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