Research On The Analysis Method Of Pesticide Multi-residue And Purification Method Of Aflatoxins In Both Chinese Materia Medicia And Its Extract

The purpose of this study is on the basis of the existing standard of Chinese Pharmacopoeia, increase the new determination items of Pesticide Residues, change the original sample preparation method to a rapid and sensitive analytical method to determinate multiple pesticide residues in CMMs. Screening the aflatoxins sample purification method which is suitable for CMMs complex matrix. Established a method to determine aflatoxins B1, B2, G1, G2in Chinese Materia Medica and pharmaceutical intermediates microbiological contaminated by immunoaffinity column clean-up combined with post-column derivatization and HPLC-FD detection. At the same time, carry out the transitivity rules of Chinese Materia Medica exogenous harmful residues of pesticides and aflatoxins in the extract of CMMs, and provide the basis for establishing limit standard of pesticide residues and aflatoxin in Chinese Materia Medica preparation.1. Research on the rapid determination method of multiple pesticide residues in CMMsFive species of CMMs, including Pinelliae Rhizoma, Angelicae Dahuricae Radix, Chuanxiong Rhizoma, Ophiopogonis Radix and Gastrodiae Rhizoma were chosen to establish the applicability of the new method. Comparison Chinese Pharmacopoeia sample preparation method and the latest QuEChERS sample preparation method. According to the complex matrix of the CMMs, chose the more suitable method for the detection of pesticide residues in Chinese Materia Medica. Besides, we modified the QuEChERS method of sample preparation to allow assay of pesticide residues in CMMs with minimal interference using GC-MS. Recovery experiments using spiked blank samples show that recoveries of the39pesticides were in the range80-120%, with RSD less than10%. Compared with other method, this modified QuEChERS method of sample preparation methods, with Quick, Easy, Cheap, Effective, Rugged and Safe, can give higher recoveries, better compatibility with GC and less interference from lipids, proteins and other co-extracted matrix components. 2. Research on the sample purification method of aflatoxins in Chinese Materia MedicaIn this paper, we using HPLC-ESI-Q-TOF-MS comparison immunoaffinity column method and solid phase extraction method, screening the aflatoxins sample purification method which is suitable for CMMs complex matrix. Solid phase extraction method in the food and agricultural products is a good purification method for aflatoxins, because it is cheap, quick and easy. However, immunoaffinity column clean-up method with highly specific monoclonal antibodies is more suitable for Chinese Materia Medica. We have established a method to determine aflatoxins B1, B2, G1, G2in Chinese Materia Medica by immunoaffinity column clean-up combined with post-column derivatization and HPLC-FD detection. The method with the great linear concentration range of0.15-6.0ng·mL-1for aflatoxins G2, B2, and0.5-20.0ng·mL-1for G1, B1respectively, was stable and accurate. The method established in this study was specific and accurate for the detection of aflatoxins in Chinese Materia Medica.3. Research on the transitivity rules of Chinese Materia Medica exogenous harmful residues of pesticides and aflatoxins in the extract of CMMsIn this paper, we studied on the transitivity rules of Chinese Materia Medica exogenous harmful residues of pesticides and aflatoxins in the extract of CMMs. We discovered that the pesticide residues in Chinese Materia Medica can’t be detected, because the destruction of boiling water or high temperature. And the aflatoxins in extract of CMMs are unable to detect may be owe to the boiling water and extraction process such as high temperature pretreatment process and the process of boiling and percolation, is bound to effect solution pH. If pH>8, aflatoxins would decompose rapidly during the extraction process. This study provided the basis for establishing standard limit of pesticide residues and aflatoxins in Chinese Materia Medica preparation.