同位素内标-高效液相色谱-串联质谱法检测常见食品样品中15种真菌毒素

Determination of 15 kinds of mycotoxins in common food by isotope internal standard-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  真菌毒素  高效液相色谱-串联质谱法  同位素内标

英文关键词:mycotoxins  high performance liquid chromatography-tandem mass spectrometry  isotopic internal standard

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的分析方法。方法 样品经乙腈-水-甲酸混合液(79:20:1, V:V:V)溶液提取后, 离心机离心, 上层清液用50%乙腈水溶液1:1稀释, 添加同位素内标后采用HPLC-MS/MS进行检测。结果 15种真菌毒素在各自范围内线性关系良好, 相关系数为0.9974~1.0000; 除串珠镰刀菌素(没有内标校正)外, 所有毒素回收率和在低、高浓度2个添加水平的回收率为72.09%~136.58%, 相对标准偏(relative standard deviation, RSD)为1.17%~27.41% (n=6), 样品定量限为1~90 μg/kg。结论 该方法快速、准确、灵敏、成本低, 适用于大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的检测。

英文摘要:

      Objective To establish a method for the determination of 15 mycotoxins in common foods such as rice, flour, corn, bean products, cakes, edible oils, meat products and fruits by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acetonitrile-water-formic acid mixture (79:20:1, V:V:V) solution, and then centrifuged. The supernatant was diluted with 50% acetonitrile water solution at 1:1. After the isotope internal standard was added, HPLC-MS/MS was used for detection. Results The linear relationships of the 15 mycotoxins were good within the range of 0.098?625 μg/L, and the correlation coefficients were 0.9974?1.0000. Except for moniliformin (without internal standard correction), the recoveries of all toxins and their recoveries at the low and high addition levels were 72.09%?136.58%, the relative standard deviation was 1.17%?27.41% (n=6), and the limits of quantitation was 1?90 μg/kg. Conclusion This method is rapid, accurate, sensitive and cheap, and is suitable for the detection of 15 mycotoxins in common food such as rice, flour, corn, bean products, cakes, edible oils, meat products and fruits.