Objective: To establish a method for determination of 7 mycotoxin contaminants in Jianqu by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods: The samples were extracted with acetonitrile aqueous solution (containing 0.1% formic acid) , and purified by QuEChERS extraction salt bag and Oasis PRiME HLB solid phase extraction column. The column of UPLC was WATERS HSS T3(100 mm×2.1 mm,1.8 μm). Mobile phase was acetonitrile-5 mmol·L-1 ammonium formate solution (containing 0.1% formic acid) with gradient elution. Ionization mode was electrospray ionization(ESI) with positive mode. The work mode was multiple-reaction monitoring mode(MRM). Results: The developed method provided a good linearity for the 7 mycotoxins with their respective linear rangers. The correlation(r) ranged from 0.999 1 to 0.999 9. The average recoveries ranged from 83.5% to 113.8%, RSDs of 2.1% to 5.2%. Among 10 samples were selected for analysis, aflatoxin B1 was detected from 3 samples at concentration of 1.32 μg·kg-1 to 6.15 μg·kg-1. The results indicated that there were serious safety risks in the Jianqu products. Conclusion: This paper establishes a method for the determination of 7 mycotoxins in Jianqu. The residual of mycotoxins in Jianqu can be rapid ly detected by UPLC-MS/MS which is suitable for the risk monitoring of mycotoxins in Jianqu. This article reveals the current situation of mycotoxins contamination in Jianqu, providing a research basis for the safety control of traditional Chinese medicine. It is recommended that the relevant departments should strengthen the corresponding supervision work.
ZHU Yuan, LU Yi-hong, WANG Jun-hu
. Rapid determination of 7 mycotoxin contaminants in Jianqu by UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(3)
: 442
-449
.
DOI: 10.16155/j.0254-1793.2024.03.09
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