同位素稀释-液相色谱-串联质谱法测定动物源性食品中6种玉米赤霉醇类化合物

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目的建立动物源性食品中6种玉米赤霉醇类化合物残留量的同位素稀释-液相色谱-串联质谱的检测方法。方法样品加入同位素内标后,用甲醇提取,离心后上清液经50℃水浴氮气吹至近干,乙酸乙酯溶解残渣后,采用氨基小柱固相萃取,正己烷-乙酸乙酯(20∶80,V/V)和乙酸乙酯两种溶液洗脱后,氮气吹干,流动相溶解后,涡旋混匀过0.22μm有机滤膜后,LC-MS/MS多反应离子监测(MRM)模式检测,内标法定量。结果 6种玉米赤霉醇类化合物在3类动物源性食品中的加标回收率为84.8%~103.6%;RSD为3.7%~8.6%;检出限和定量限分别为0.03~0.07μg/kg和0.10~0.24μg/kg。结论该方法灵敏、准确,适用于动物源性食品中玉米赤霉醇类物质的检测。 Objective To establish a method for the determination of 6 zearalenol residues in animal derived products by isotope dilution - liquid chromatography - tandem mass spectrometry. Methods The sample was extracted with methanol after adding isotope internal standard. After centrifugation, the supernatant was blown to near dryness by nitrogen atmosphere at 50 ℃. The residue was dissolved in ethyl acetate, 80, V / V) and ethyl acetate. After the mobile phase was dissolved in the mobile phase, the mixture was vortexed and mixed with 0.22 μm organic membrane. LC-MS / MS MRM Pattern detection, internal standard method. Results The spiked recoveries of six kinds of zearalenol in three kinds of animal derived foods ranged from 84.8% to 103.6% with RSD from 3.7% to 8.6%. The detection limits and the limits of quantification were 0.03-0.07 μg / kg and 0.10 to 0.24 μg / kg. Conclusion The method is sensitive and accurate and is suitable for the detection of zearalenol in animal derived foods.
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