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Analytical Technologies For Hazardous-Chemical Detection In Honey And E'jiao

Posted on:2021-04-15Degree:MasterType:Thesis
Country:ChinaCandidate:S ZhangFull Text:PDF
GTID:2381330620967019Subject:Applied Chemistry
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Honey and E'jiao are two important medicine and food dual purposes products.The safety of these two products have been widely concerned by consumers.This paper established a high-resolution mass spectrometers library for multiple potentially harmful compounds by ultraperformance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS).Then,the ultrahigh performance liquid chromatography-triple quadrod mass spectrometry(UPLC-MS/MS)methods were develoed for analysis of phytotoxins in honey and pesticides in Ejiao.Details are as follows:A comprehensive mass spectra based library of 590 chemical hazardous,including natural toxins,illegal adulterants,pesticides,veterinary drugs and contaminants,was constructed using UPLC-QTOF-MS,and then proper pretreatment procedures was considered for the preparation of honey and E'jiao.A preliminary QuEChERS pretreatment procedures was developed for rapid highthrough-put screening of chemicals.An UPLC-MS/MS mehod was estabolised for the simultaneous determination of 18 phytotoxins,including tripterygium alkaloids,pyrrolizidine alkaloids,isoquinolines,corianin and tutin,in honey.Acetonitrile extraction,QuEChERS and other pretreatment process were compared.Matrix-matched external standard calibration curve was utilized for quantification.Method validation included limit of detection(LOD),lower limit of quantitation(LLOQ),linearity,precision and recovery was evaluated.The method resulted in good linearity(R~2?0.99)for all of the phytotoxins and LOQ ranging from 0.002?g/L to 0.7?g/L except nuciferine and tutin is 2 and 4?g/L respectively.The mean recoveries of all detected compounds were 70~112%at three levels of spiked concentration,only the recoveries of lycopsamine was 48~60%.The method provides an efficient strategy for simultaneously qualitative analyzing multiple types phytotoxin in honey.An UPLC-MS/MS mehod was estabolised for the simultaneous determination of 281 pesticides in E'jiao.By comparing the sample pretreatment method of QuEChERS and comparing the purification effects of C18,PSA,Z-sep+and other adsorbents,Z-sep+was proved the optimal.Recoveries for 70%of the compounds were above 60%and the detection limit of 80%compounds was below 1?g/L.This method can satisfy the needs of high-throughput detection of pesticides in E'jiao.
Keywords/Search Tags:honey, E'jiao, ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS), high-resolution mass spectrometry, QuEChERS, phytotoxin, pesticide, screening
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