Study On The Pesticide Multi-residue Of Jiawei Xiaoyao Tablets And Its Prescription Chinese Medicinal Materials

Objective:Recently,the growing demand for traditional Chinese medicine has prompted,most commonly used Chinese medicinal materials were converted to artificial scale cultivation.Pesticides are inevitably used in the cultivation of traditional Chinese medicine,which may cause serious health and environmental pollution issues.Various countries have successively added strict limit requirements for pesticide residues in Chinese medicinal materials.Therefore,it is significant to comprehensively understand the status of pesticide residues in Chinese medicinal materials.In this study,232 pesticide residues are selected as detection indicators.Jiaweixiaoyao pills,six herbs in its prescription and two extracts are selected as research objects,such as Angelicae Sinensis Radix,Bupleuri Radix,Paeoniae Radix Alba,Atractylodis Macrocephalae Rhizoma,Poria and Glycyrrhizae Radix et Rhizoma,and 2 extracts,including extract of Angelicae Sinensis Radix,Atractylodis Macrocephalae Rhizoma.and Glycyrrhizae Radix et Rhizoma;extract of Bupleuri Radix and Paeoniae Radix Alba.Pesticide multi-residue detection methods which were used to screen the samples mentioned above were established in this thesis in order to obtain the situation of pesticide residues and to investigate the transfer of pesticide residues in the preparation process.Methods:1.Selection of pesticide residues.Because the import and export of Chinese medicinal materials in China is affected by the detection of pesticide residues,and many countries in the world use the pesticide residue limit standards stipulated in the European Pharmacopoeia as the basis,232 pesticide detection indicators were determined based on the actual use of pesticides in China and the pesticide residue indicators in the European Pharmacopoeia.2.Establishment of three pesticide multi-residue detection methods:GC-MS/MS,LC-MS/MS,GC.GC is the exclusive detection method for dithiocarbamate pesticide residues,and detected pesticide residues in samples.3.Established 4 kinds pre-treatment method of 9 matrices,including 6 Chinese herbal medicines,2 extracts,1 preparation.Targeting different types of matrices,this study used different purification method,such as using direct injection without purification,and different types and proportions of dispersed powder purification.These methods can reduce matrix interference,make measurement results accurate and reliable,as well as simplify experimental operations.4.This study detected pesticide residues in 36 batches of the traditional Chinese medicine mentioned above.Result:1.GC-MS/MS,LC-MS/MS and GC detection methods for pesticide multi-residue are successfully established.GC-MS/MS and LC-MS/MS detection methods have a good linear relationship.The average recoveries at spiked 3 levels(0.01 mg·kg-1?0.1 mg·kg-1 and 0.5 mg·kg-1),the 94%average recovery was 70-120%,RSD overall ?7%.The linear relationship between GC for dithiocarbamate pesticide detection method is a quadratic equation,r2=1.0000,the average recovery was 99%-1 15%,RSD 2.0%.All met the requirements for trace pesticide residue detection.2.Pretreatment methods for 4 different matrixes are successfully established in this thesis,eliminating the interference and influence of matrix effect on experimental results.3.According to pesticide residue detection on the traditional Chinese medicine mentioned above,there are 13 pesticide residues were detected which accounts for 5.60%of all pesticides tested.The test result is that seven common pesticides detected met the Chinese and European standards,and among six pesticides required by the European Pharmacopoeia,except the amount of heptachlor detected in a batch of Paeoniae Radix Alba exceeded the limit,rest of pesticides meet the requirements of the limit standard.Generally speaking,low levels of pesticide residues were detected in only a few batches in the sample in which the biggest amount of pesticides were detected from Atractylodis Macrocephalae Rhizoma,thus it basically met the requirements of the limit standard.Conclusion:This study established an efficient and accurate methods for the detection of pesticide residues and pretreatment methods that can be used for the detection of multiple pesticide residues.The method with high sensitivity,accuracy and reliability enabled the test results to provide a reference for the formulation of pesticide residue standards.