The Rearch Of Detection On Mycotoxins Contaminants In Foods By QuEchERS Combined With LC-MS/MS

Mycotoxins have toxic effects on humans,such as teratogenicity,carcinogenesis,and mutagenesis.Foods can be easily contaminated by mycotoxin in the supply chain because of improper storage conditions.To ensure food safety,the monitoring of mycotoxin contamination is very important,and various techniques have been used for the detection of mycotoxins.QuEChERS technology is one of the most important methods which has the characteristics of quick,easy,cheap,effective,rugged,and safe.It has been widely used to detect mycotoxin in recent years.In this study,a rapid detection method of aflatoxin B₁,B₂,G₁,G₂ and ochratoxin A,B,and C in foods was established using QuEChERS pretreatment combined with high performance liquid chromatography-mass spectrometry.The method is high sensitivity and good reproducibility,which is suitable for high-volume sample screening.The main research content is as follows:1?Methods were developed to detect three ochratoxins contaminants including ochratoxin A?OTA?,ochratoxin B?OTB?and ochratoxin C?OTC?)in wine via a combination of QuEChERS technology and high performance liquid chromatography?HPLC?and tandem Mass Spectrometry?HPLC-MS/MS?.The wine samples were diluted with acetonitrile-glacial acetic acid?90:10,V/V?and then purified with a modified QuEChERS technology using a scavenging agent combination of C₁₈,SiO₂and MgSO₄ after centrifugation.The separation was performed on C₁₈8 column?4.6mm×250 mm,5?m?after the gradient elution on a liquid chromatography.Three ochratoxins contaminants in wine were analyzed by HPLC-FLD and LC-MS-MS in the positive ionization under the multiple-reaction monitoring?MRM?mode.By these methods,the limit of quantification?LOQ?were 2.0?g/kg and the relative standard deviation?RSD?was between 2.01%and 7.52%?n=6?.Conclusion The developed methods proved to be simple,sensitive,reproducible and were suitable for the determination of ochratoxins in wine in daily supervision work.2?A simple,fast,economic and highly sensitive detection method of seven kinds of mycotoxins including Aflatoxin B₁?AFB₁?,Aflatoxin B₂?AFB₂?,Aflatoxin G₁?AFG₁?,Aflatoxin G₂?AFG₂?,Ochratoxin A?OTA?,Ochratoxin B?OTB?and Ochratoxin C?OTC?in food was developed.The samples were diluted with acetonitrile-formic acid?90+10,V/V?and then purified with a modified QuEChERS technology using a scavenging agent combination of C₁₈,Al-N,PSA and MgSO₄ after centrifugation.The separation was analyzed by LC-MS/MS in the positive ionization under the multiple-reaction monitoring?MRM?mode.Limits of quantitation?LOQs?were 0.25².0?g/kg and the relative standard deviations?RSD,n=6?were between1.1%and 7.7%.The developed method was proved to be simple,sensitive,and reproducible and was suitable for the determination of these ochratoxins in foods in daily supervision work.3?To select a more suitable pretreatment method for different types of food,the five food matrices were cleaned up with different pretreatment methods and detected by LC-MS/MS.After pre-treatment with a conventional QuEChERS and a new purification method called Bond Elut Enhanced Matrix Removal-Lipid?EMR-Lipid?,high performance liquid chromatography?HPLC?and high performance liquid chromatography-tandem Mass Spectrometry?LC-MS/MS?were used respectively to detect seven mycotoxins in five food matrices.Comparison of recoveries,purification effects and detection costs of conventional two purification methods were carried out.The results show:EMR-Lipid purification method is superior to the conventional QuEChERS purification method in pretreatment with oil-rich food matrices.Considering the detection cost and efficiency,the conventional QuEChERS purification method can be selected for large-scale determination of samples.