| Objective:The pretreatment methods and matrix have a great impact on the determination results of pesticide residues in different Chinese medicinal materials.This paper studies the optimization of different pretreatment methods,the selection of new purification materials,the detection and risk assessment of multiple pesticide residues in Anhui grown Chinese medicinal materials.This paper aims to provide a reference for the selection and optimization of pretreatment methods for the detection of 33 banned pesticide residues in different Chinese medicinal materials,and improve the detection efficiency.Taking Anhui real estate medicinal materials as the research object,the method system of pesticide multi-residue detection in Chinese medicinal materials was established and preliminary risk assessment was carried out,which could provide reference for quality safety and risk management of Anhui grown Chinese medicinal materials.Methods:1.Study on the pretreatment methods for the residue detection of 33 banned pesticides in different matrix Chinese medicinal materials based on the 4th edition of the "Pharmacopoeia of the People’s Republic of China"(hereinafter referred to as the "Pharmacopoeia of China")2020 edition(1)Review literatures related to pesticide residues and conduct field research,and finally select 31 varieties of Chinese medicinal materials covering different medicinal parts of roots,rhizomes,flowers,leaves,fruits and skins.(2)31 varieties of Chinese medicinal materials were taken as research objects,recovery rates of 33 prohibited pesticides were taken as evaluation indexes,and the effects of 3 categories(5 in total)of pretreatment methods in the four volumes of the2020 edition of Chinese Pharmacopoeia on the detection of 33 prohibited pesticide residues were compared from different substrates,different extraction methods and different purification methods.2.Optimize the pretreatment method of 33 banned pesticide residues detection in traditional Chinese medicinal materials with complex matrix(1)Optimization of pretreatment methods of Chinese medicinal materials containing more pigments The recovery rate of 33 banned pesticides was used as the evaluation index to investigate the optimized pretreatment method from the aspects of extraction method,matrix effect and recovery rate,respectively.(2)Study on new pretreatment materials of Chinese medicinal materials with higher volatile oil content The recovery rate of 33 banned pesticides was taken as the evaluation index,and the types and amounts of purification fillers were investigated to screen out the purification fillers suitable for Chinese medicinal materials with high volatile oil content.3.To establish a method for pesticide residue detection of Anhui grown Chinese medicinal materials.Five kinds of traditional Chinese medicinal herbs(Gastrodia elata,Pseudostellariae Radix,Chaenomelis Fructus,Thesii Herba and Clnopodii Herba)from Anhui grown Chinese medicinal materials were selected as the research objects.By combining field investigation and literature review,111 kinds of pesticides were selected as detection indexes,matrix effect,purification effect and recovery rate were taken as evaluation indexes,and the pre-treatment methods of pesticide multi-residue detection for 5 kinds of Anhui grown Chinese medicinal materials were studied from two aspects of extraction and purification.Combined with LC-MS/MS method and GC-MS/MS method,a method for the analysis of 111 kinds of pesticide residues in 5 kinds of Chinese medicinal materials was established.4.Study on risk assessment of traditional Chinese medicine in Anhui grown Chinese medicinal materials The established method was used to detect 111 pesticide residues in 87 batches of Anhui grown Chinese medicinal materials.According to the experimental data of pesticide residues of each variety,the Hazard Quotient(HQ)and Hazard Ibdex(HI)were used to evaluate the residue risk.Results:1.Study on the pretreatment methods for the residue detection of 33 banned pesticides in different matrix Chinese medicinal materials based on the "Pharmacopoeia of the People’s Republic of China"(2020 Edition IV)Through the comparison and study of three categories and five pre-treatment methods specified in the four parts of the Chinese Pharmacopoeia 2020 Edition,it was found that 81% of the 31 kinds of Chinese medicinal materials,most of which has pesticide recoveries within 60%~130% and meet the detection requirements.2.Optimize the pretreatment method of 33 banned pesticide residues detection in traditional Chinese medicinal materials with complex matrix(1)Optimization of pretreatment methods of traditional Chinese medicine containing more pigments The optimized method was used to detect 33 prohibited pesticide residues in Salvia miltiorrhiza Radix et Rhizoma.It was found that 33 prohibited pesticides in Salvia miltiorrhiza Radix et Rhizoma had a good linear relationship at a certain concentration,r was greater than 0.9900,and the RSD was less than 15% when the recovery rate was64.43%~127.35%,meeting the detection requirements.(2)Research on new pretreatment materials of traditional Chinese medicine with high volatile oil content By investigating the effects of PSA,C18,multi-walled carbon nanotubes and EMR fillers on the recovery rates of 30 kinds of banned pesticides detected by LC-MS/MS,it was found that EMR fillers were suitable for the detection of 30 kinds of banned pesticides.The pesticide recoveries were 64.2%~103.0% and RSDS were1.18~12.89%,which met the detection requirements.3.To establish a method for pesticide residue detection of traditional Chinese medicinal materials in Anhui province According to the classification of matrix characteristics,the pesticide residue analysis methods represented by Gastrodia elata and Thesii Herba were established.Taking by Gastrodia elata as the representative,111 pesticides were detected by the established analytical method(including 81 pesticides detected by LC-MS/MS,44 pesticides detected by GC-MS/MS,14 pesticides that can be detected by LC-MS/MS and GC-MS/MS).The recovery rate of 81 pesticides detected by LC-MS/MS was73.0%~122.2%,and the RSD was 0.65%~9.05%;The recoveries of 44 pesticides detected by GC-MS/MS were 61.2%~119.9%,and the RSD was 0.86%~12.78%.Taking by Thesii Herba as the representative,The results showed that the recoveries of81 pesticides detected by LC-MS/MS were 61.00%~128.6%,and the RSD was1.49%~13.61%;The recoveries of 44 pesticides detected by GC-MS/MS were60.7%~129.7%,and the RSD was 0.53%~7.22%,meeting the detection requirements.4.Results of pesticide multiple residue detection and risk assessment of 5 kinds of traditional Chinese medicinal herbs in Anhui province A total of 111 pesticides were tested for 5 kinds of traditional Chinese medicinal herbs(87 batches)from Anhui province.A total of 1 pesticide was detected in 14 batches of Gastrodia elata;Six pesticides were detected in 14 batches of Pseudostellariae Radix,and the detection rate of 9 batches was 64.29%;9 kinds of pesticides were detected in 14 batches of Chaenomelis Fructus and 6 batches of samples,with the detection rate of 42.86%;14 pesticides were detected in 18 batches of Thesii Herba,and 11 batches of samples were detected,with the detection rate of 61.11%;12pesticides were detected in 13 batches of severed Clnopodii Herba and 10 batches of samples,with a detection rate of 76.92%.Although many pesticides have been detected in the above five Chinese medicinal materials,the HQ and HI values are less than 1,and the risk is considered acceptable.Conclusion:1.This paper summarized the characteristics of 5 pretreatment methods for 33 banned pesticide residues detection in the fourth volume of Chinese Pharmacopoeia(2020edition),and recommended the best pretreatment methods for 33 banned pesticide residues detection in 31 Chinese medicinal herbs.2.Optimization of pretreatment methods for 33 banned pesticide residues detection of Chinese medicinal herbs with complex matrix.(1)Optimization of pretreatment methods for Chinese medicinal herbs with more pigments.The optimized Qu ECh ERS method is fast and simple,which provides a reliable detection method for routine detection of 33 banned pesticide residues in Salvia miltiorrhiza Radix et Rhizoma,and provides a reference for the determination of 33 banned pesticide residues in similar matrices with more pigments.(2)At the same time,the new pretreatment materials of Chinese medicinal materials with high volatile oil content were studied,and it was found that the new purification filler EMR had the best effect on the removal of impurities in Hansenia weberbaueriana(Fedde ex H.Wolff)Pimenov,which provided the idea for the determination of 33 kinds of prohibited pesticide residues in Chinese medicinal materials with high volatile oil content.3.The method of pesticide multiple residue analysis established for 5 kinds of Anhui birth canal medicinal materials is accurate,reliable and reproducible,which can provide an important basis for the quality evaluation of 5 kinds of medicinal materials.To assess the risk of pesticides detected in samples,and to provide reference for monitoring the quality safety and risk management of local medicinal materials in Anhui province. |
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