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Study On Rapid Screening And Quantitative Analysis Pesticide Residues In Medical And Edible Plants By GC/MS-MS And UHPLC-MS/MS

Posted on:2016-04-10Degree:MasterType:Thesis
Country:ChinaCandidate:Z ChengFull Text:PDF
GTID:2271330461454451Subject:Agricultural Products Processing and Storage
Abstract/Summary:PDF Full Text Request
The medical and edible plants, such as ginseng, Lycium barbarum L has a long application history in our country which has been associated with in People’s Daily life and at the same time medical and edible plants is also an important component treasure of the Chinese nation-Chinese medicine. Traditional Chinese medicinal herbs also have been the important tool of our people’s disease cure which has played a huge role to safeguard the people health and thriving of the Chinese nation. In recent years, in order to improve the yield and economic value, various types of pesticides use to process of cultivation, which can cause pesticide residue problems.With the outbreak of the security events, food and drug safety problems aroused more and more people’s attention, the problem of pesticide residue is very important part among them. To a certain extent pesticide residue affects the modernization and internationalization of Chinese herbal medicine industry, also affects our country’s reputation of Chinese herbal medicine in the international market. An analytical method for the simultaneous determination of almost 160 pesticide residues in traditional Chinese medicinal herbs was established based on optimized Qu ECh ERS as a former processing technology, combined with gas chromatography-tandem mass spectrometry(GC/MS-MS) and ultra-high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS). This simple, rapid, sensitive, accurate and high-throughput method achieved satisfactory results, can be applied to the target screening of these pesticide residues in real samples. Specific content is as follows:①An analytical method for the simultaneous determination of 144 pesticide residues in traditional Chinese medicinal herbs was established based on optimized Qu ECh ERS with gas chromatography-tandem mass spectrometry(GC-MS/MS).The influences of different extraction solvents, different buffer systems and different purifying agents on the recoveries of pesticides were investigated. The pesticide residues from the samples were extracted with acetonitrile, and then cleaned up by the mixed sorbents to GC/MS-MS in multi-reaction monitoring(MRM) mode. The external standard method was applied to quantify the pesticides. The linearity of the method was in the range of 20 to 2000 μg/kg with correlation coefficients(r2) of more than 0.983.The recoveries of the pesticides at the spiking levels of 20, 50, and 200μg/kg ranged from 74.3% to111.8% with relative standard deviations lower than 15%, except for acephate, amitraz and aldrin.The method was successfully used for the analysis of target pesticides in testing samples, and had a good consistency with the existed standard one. This multi-residue analytical method allows for a rapid, efficient, sensitive and reliable screening and quantitative analysis of target pesticides in traditional Chinese medicinal herbs.②A modified Qu ECh ERS followed by ultra-high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS) under the dynamic multiple reactions monitoring(d MRM) mode was used for the analysis of 85 pesticide residues in two typical traditional Chinese medicinal herbs(TCMHs): honeysuckle and ginseng. The method was validated by a recovery test at three spiking concentrations of 20, 50 and 200 μg·kg-1(n=4). The majority of recoveries ranged from70% to 120%with RSDs less than 15%. With the matrix-matched quantification calibration, the developed method showed a good linear dynamic range with regression coefficients(r2) of 0.99 or higher. This method allowed for detection of the 85multi-class pesticide residues with LOQs significantly lower than the current maximum residue levels(MRLs) regulated by China, USA and EU. This simple, rapid, sensitive, accurate and high-throughput method can be applied to the target screening of these pesticide residues in real samples.③Using the above two detecting methods, detect ginseng, Lycium barbarum L, American ginseng, poriacocos, rhizome atractylodis macrocephalae, radixbupleuri, cortex moutan which Gathered in Beijing, tianjin, Yunnan and some other places. Sample collection period is 2013-2014, sample amounted to nearly 500. Through the screening of the sample, the analysis of the data sorting, find out high residual rate of Chinese herbal medicine and pesticide target analyte. This data accumulation and summarized to provide the basis for the safety of Chinese herbal medicine.
Keywords/Search Tags:GC-MS/MS, Pesticide residues, Traditional Chinese medicinal herbs, Qu ECh ERS, UHPLC-MS/MS, d MRM
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