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    QuEChERS-超高效液相色谱-串联质谱法测定茶叶中伏马毒素B1、B2、B3的含量

    Determination of Fumonisins B1, B2 and B3 in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS

    • 摘要: 茶叶样品经粉碎、过筛后,分取2.50 g,加入2.0 mL水润湿,再加入20 mL含1%(体积分数)甲酸的乙腈溶液,涡旋3 min,在4℃下离心10 min。分取1.0 mL上清液,置于含有净化剂(250 mg无水硫酸镁和150 mg多壁碳纳米管)的2.0 mL离心管中,涡旋3 min,在4℃下离心10 min。收集上清液,过0.22 μm有机相滤膜,弃去初滤液,续滤液用超高效液相色谱-串联质谱法分析。进行色谱分析时,以Agilent Poroshell 11色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈的混合溶液作流动相进行梯度洗脱分离。进行质谱分析时,以电喷雾离子源正离子(ESI+)模式电离,多反应监测(MRM)模式检测。结果显示:伏马毒素B1、B2、B3的质量浓度在0.5~100.0 μg·L-1内和对应的峰面积呈线性关系,检出限(3S/N)为0.15~1.00 μg·kg-1。按照标准加入法进行回收试验,回收率为82.1%~108%,测定值的相对标准偏差(n=6)为2.7%~5.3%。方法用于50批茶叶样品的分析,在一批黑茶样品中检出了伏马毒素B1,检出量为8.321 μg·kg-1

       

      Abstract: After crushing and sieving the tea sample, an aliquot (2.50 g) was taken, and 2.0 mL of water was added for wetting. Then 20 mL of acetonitrile solution containing 1% (volume fraction) formic acid was added, and the mixture was vortexed for 3 min, and centrifuged at 4℃ for 10 min. An aliquot (1.0 mL) of the supernatant was taken and placed into a 2.0 mL-centrifuge tube containing the purifiers (250 mg of anhydrous magnesium sulfate and 150 mg of multiple walled carbon nanotubes). The mixture was vortexed for 3 min, and centrifuged at 4℃ for 10 min. The supernatant was collected, and passed through a 0.22 μm organic phase filter membrane. The initial filtrate was discarded, and the subsequent filtrate was analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry. In chromatographic analysis, Agilent Poroshell 11 chromatographic column was used as the stationary phase, and mixed solutions composed of 0.1% (volume fraction) formic acid solution and acetonitrile at different volume ratios were used as the mobile phase for gradient elution separation. In mass spectrometry analysis, electrospray ion source positive ion (ESI+) mode was used for ionization, and multiple reaction monitoring (MRM) mode was used for detection. It was shown that linear relationships between values of the mass concentration of fumonisins B1, B2, and B3 and the corresponding peak area were kept in the range of 0.5-100.0 μg·L-1, with detection limits (3S/N) in the range of 0.15-1.00 μg·kg-1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 82.1%-108%, and RSDs (n=6) of the determined values ranged from 2.7% to 5.3%. The proposed method was used for the analysis of 50 batches of tea samples, and fumonisin B1 was detected in a batch of black tea sample, with detection amount of 8.321 μg·kg-1.

       

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