The Study Of The Methods For The Hplc Determination Of Deoxynivalenol In Black Pepper

The establishment of determination methods of deoxynivalenol in black pepper was systermaticly researched and the conditions of extraction, purification and HPLC detection were optimized in the thesis. The determination methods of organic solvant extraction-IAC purification-HPLC detection, water extrction-IAC purification-HPLC detection and extraction-MycoSep227 multifunctional column purification-HPLC detection were studied to detect DON in black pepper, respectively. The main results of the study are concluded as below.1. The determination method of organic solvent extraction-IAC purification-HPLC detection was developed. The limit of detection(LOD) and the limit of quantitation(LOQ) of DON were 10μg/kgå'Œ33μg/kg, respectively. Recoveries of DON spiked at levels of 0.5～2μg/g ranged from 72.68% to 91.47%, with RSD less than 3, which met the requirements of the determination. Precision and reproducibility were fine.2. The most conformable determination method of DON in black pepper was developed, which was water extraction-IAC purification-HPLC detection. The LOD and LOQ of DON were 14μg/kg and 55μg/kg, respectively.The average recovery was 103.88%, and the RSD ranged from 1.73 to 2.45. Compared with organic solvent extraction method, water extraction method reduced the transfer operations and used the two-step extraction to effectively expand the contact area between material and liquid. The recovery and the reproducibility of water extraction were both better than the organic solvent extraction.3. The determination method of DON in black pepper, which was extraction-MycoSep227 multifunctional column purification-HPLC detection, was developed.The LOD and the LOQ were 50μg/kg and 200μg/kg, respectively. Recoveries of DON spiked at levels of 0.2～4μg/g ranged from 89.66% to 98.78%, with RSD between 1.81 and 3.25. Compared with IAC, the purification effect and the reproducibility of MycoSep227 multifunctional column were poor. Especially when the DON content was lower, excessive impurities of DON would seriously interfere the detection of HPLC.