To establish a method for determination of 7 mycotoxin contaminants in Jianqu by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).
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).
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.
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.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |