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| Determination of fumonisins B1 and B2 in maize by improved QuEChERS-UPLC-QTRAP-MS/MS technique |
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| KeyWord:improved QuEChERS UPLC-QTRAP-MS/MS maize fumonisin |
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| Abstract: |
| The sample preparation method of QuEChERS was improved to provide a good analytical result for the determination of fumonisins B1 and B2 in maize with UPLC-QTRAP-MS/MS. The samples were shakingly extracted with acidified acetonitrile aqueous solution, after liquid-liquid partition using MgSO4 and NaCl, the supernatant was purified using MgSO4, PSA, C18, graphitized carbon black and neutral alumina as adsorbing material,then separation of fumonisins B1 and B2was performed with C18 column. The mobile phase gradiently eluted with methanol and 0.1% formic acid aqueous solution. The electrospray was operated in the positive ionization mode and two kinds of fumonisins were identified by multi-reaction detection (MRM)-information dependent acquisition (IDA)-enhanced production ion (EPI) scan mode. Qualitative analysis was performed by online EPI spectrum library search, and quantification was conducted by external standard method. The results showed that the calibration curves showed good linearity within the mass concentration of 10-500 μg/L with the correlation coefficients all above 0.999. The detection limits for fumonisins B1 and B2 were 5 μg/kg and 3 μg/kg respectively. The recoveries of two kinds of fumonisins were 8911%-104.61% at low, medium and high levels of addition,and the relative standard deviation were 2.33%-989%. Compared with immunoaffinity column method, the recoveries and specificity of the two methods were not much different, but the improved QuEChERS method had more advantages in analytical time and cost. |
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