超高效液相色谱串联质谱测定常见农产品中40种真菌毒素

Simultaneous determination of 40 mycotoxins in common agricultural products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  真菌毒素  农产品

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  mycotoxins  agricultural products

中文摘要:

      目的 建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测小麦、玉米、稻谷、番茄和桃等常见农产品中40种真菌毒素含量的分析方法。方法 谷物样品先后经水和含1%(V/V)甲酸的乙腈溶液提取, 果蔬样品经1%(V/V)甲酸的乙腈溶液提取, 氯化钠和无水硫酸镁盐析后, 取上清液氮吹至干, 残渣经5 mmol/L醋酸铵水溶液-乙腈(80:20, V/V)复溶, 过膜后上机测定, 通过基质匹配标准曲线进行定量分析。结果 40种真菌毒素在各自的线性范围内线性关系良好, 相关系数(r2)≥0.99, 检出限和定量限分别为 0.2~10.0 μg/kg 和 0.5~20.0 μg/kg。在低、中、高3个添加水平下, 5种农产品基质中40种真菌毒素的平均加标回收率为71.8%~118.6% 精密度为1.2%~16.9%(n=5)。结论 本方法操作简单、灵敏度高、实用性强, 适用于小麦、玉米、稻谷、番茄和桃等常见农产品中40种真菌毒素的同时检测分析。

英文摘要:

      Objective To establish an analytical method for simultaneous determination of 40 mycotoxins in different agricultural products (wheat, maize, rice, tomato and pench) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The grain samples were extracted with water and acetonitrile containing 1% (V/V) formic acid. and tomato and peach samples were extracted with acetonitrile containing 1% (V/V) formic acid. After salted out with sodium chloride and anhydrous magnesium sulfate, an aliquot of the supernatant was dried by nitrogen gas, re-dissolved by 1 mL water containing 5 mmol/L ammonium acetate-acetonitrile (80:20, V:V), filtrated and analyzed by UPLC-MS/MS. Accurate quantification was achieved by matrix-matched calibration curves. Results. Good linear relationships were obtained in respective linear ranges and the correlation coefficients (r2) were greater than 0.99. The limits of detection and the limits of quantification in different matrices ranged from 0.2?10.0 μg/kg and from 0.5?20.0 μg/kg, respectively. Recoveries of 40 kinds of mycotoxins in five kinds of agriculture products at low, medium and high spiked levels were ranged from 71.8%?118.6% (n=5), with precisions in the range of 1.2%?16.9%. Conclusion This method is simple, rapid and practical, which is suitable for quantitative analysis of 40 kinds of mycotoxins in various agricultural products.