药食同源中药材中16种真菌毒素的测定与分析

目的:建立同位素标记-超高效液相色谱-串联质谱法(UPLC-MS/MS)测定药食同源中药材中16种真菌毒素的分析方法,并利用该方法对市售的483份药食同源样品进行检测分析.方法:样品用乙腈-水(50/50,V/V)提取,MycoSpinTM 400多毒素净化柱净化,经Acquity UPLC BEH C18色谱柱(10...

Determination and Analysis of 16 Mycotoxins in Medicinal and Edible Traditional Chinese Medicine

Objective: An analytical method was established for the determination of 16 mycotoxins in traditional Chinese medicines (TCM) by isotope labeling-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS), and 483 medicinal and edible homologous samples from the markets were detected using this method. Method: The samples were extracted with acetonitrile-water (50/50, V/V), and then purified by the MycoSpinTM 400 multifunction clean-up columns. Then the samples were detected and confirmed by UPLC-MS/MS, and quantified by isotope labeled internal standards. Rapid separation of 16 mycotoxins was successfully achieved on an Acquity UPLC BEH C₁₈ column（100 mm×2.1 mm, 1.7 μm）with gradient elution. Simultaneous acquisition was performed in multiple reaction monitoring (MRM) mode with electrospray ionization (ESI) source operated in both positive and negative ionization modes. Result: The established method provided good linearities for the 16 mycotoxins within their respective linear ranges with high correlation coefficients (R>0.998), and the detection limits of this method were 0.1~4.0 μg/kg. The average recoveries of the 16 mycotoxins ranged from 83.4% to 102.3% at the three spiked levels, and the relative standard deviations (RSD, n=6) were in the range of 2.08%~13.6%. In the detection of 483 actual samples, 10 mycotoxins were detected, and the other 6 mycotoxins were not detected. The toxin compound with the highest detection rate was zearalenone (ZEN), with an average content of positive samples 71.2 μg/kg, and 3.11% of the samples exceeded the reference limit specified in the national food safety standard. Conclusion: This method used isotope dilution and multifunction clean-up columns to purify the samples, which reduced the matrix interference in the medicinal and edible homologous samples. The detection limits could meet the requirement of methods. The method was accurate and rapid, and could be used for the detection and analysis of multi residues of mycotoxins in a large number of samples.