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| 改良QuEChERS法结合UPLC-QTRAP-MS/MS技术测定玉米中的伏马毒素B1 、B2 |
| Determination of fumonisins B1 and B2 in maize by improved QuEChERS-UPLC-QTRAP-MS/MS technique |
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| DOI： |
| 中文关键词: 改良QuEChERS UPLC-QTRAP-MS/MS 玉米 伏马毒素 |
| 英文关键词:improved QuEChERS UPLC-QTRAP-MS/MS maize fumonisin |
| 基金项目: |
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| 中文摘要: |
| 改进QuEChERS样品制备方法，为玉米中伏马毒素B1、B2的UPLC-QTRAP-MS/MS检测提供良好的分析结果。该方法包括将样品与酸化的乙腈水溶液混合振荡提取，然后使用MgSO 4、NaCl进行盐析液体分配，通过用MgSO 4、PSA、C18、石墨化碳黑和中性氧化铝分散固相萃取净化，C18色谱柱分离，以甲醇-0.1%甲酸水溶液为流动相梯度洗脱，正模式扫描，采用多反应检测（MRM）-信息依赖采集（IDA）-增强子离子扫描（EPI）模式检测，在线EPI谱库定性分析，外标法定量。结果表明：在10~500 μg/L的质量浓度范围内，2种伏马毒素的线性相关系数均大于0.999，检出限分别为5 μg/kg和3 μg/kg；添加低、中、高3个水平，2种伏马毒素的平均回收率在89.11%~10461%之间，相对标准偏差在2.33%~9.89%之间。与免疫亲和柱法比较发现，两种方法的回收率和特异性差别不大，但是改良的QuEChERS方法更具有时间和成本效益。 |
| 英文摘要: |
| 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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