高效液相色谱-串联质谱法测定米粉中8种真菌毒素

Determination of 8 kinds of fungal toxins in rice noodles by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  米粉  真菌毒素

英文关键词:high performance liquid chromatography-tandem mass spectrometry  rice noodles  fungal toxins

中文摘要:

      目的 建立一种液液分散-净化柱处理, 高效液相色谱-串联质谱法同时测定米粉中8种真菌毒素的分析方法。方法 米粉样品中加入同位素内标, 用乙腈-水(80:20, V:V)振荡提取25 min, 液液分散萃取, 多功能净化柱净化, 采用HSS T3液相色谱柱分离待测物, 以乙腈-水(0.1%甲酸)为流动相, 进行梯度洗脱。采用电喷雾离子化, 正、负离子扫描, 多重反应监测模式, 保留时间和特征离子对定性, 内标法定量。结果 该方法检测8种真菌毒素在对应的范围内线性关系良好, 线性相关系数(r)为0.9954~0.9998, 方法检出限为0.10~10.00 μg/kg, 定量限为0.30~30.00 μg/kg。分别测定低、中、高3种添加水平的加标样品, 回收率为75.8%~112.0%, 相对标准偏差为2.9%~5.9%。对市售的21种米粉样品中的8种真菌毒素进行检测分析, 除HT-2外7种毒素均有检出。结论 本方法样品前处理步骤简单, 检测结果精密准确、灵敏度较好, 适用于米粉中8种真菌毒素的检测。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of fungal toxins in rice noodles with liquid-liquid dispersion extraction and multifunctional purification by high performance liquid chromatography-tandem mass spectrometry. Methods Rice noodle samples were added with isotopic internal standards, and extracted by shaking with acetonitrile water (80:20, V:V) for 25 min. After liquid-liquid dispersion extraction, a multifunctional purification column was used for purification. The 8 kinds of target compounds were separated on HSS T3 column, with acetonitrile-water (0.1% formic acid) used as the mobile phase for gradient elution, and detected under positive and negative ionization and multiple reaction monitoring mode, determined with retention time and characteristic ion pairs, quantified with internal standard method. Results This method had a good linear relationship in detecting 8 kinds of fungal toxins within the corresponding range. The correlation coefficients (r) of the target compounds were 0.9954–0.9998. The limits of detection were 0.10–10.00 μg/kg, and the limits of quantification were 0.30–30.00 μg/kg. The average recoveries of rice noodle samples at low, middle and high standard additions were 75.8%–112.0%, and the relative standard deviations were 2.9%–5.9%. The detection and analysis of 8 kinds of fungal toxins in 21 kinds of rice noodle samples in the market showed that all the toxins were detected except HT-2. Conclusion The pretreatment of sample is simple, the method is accurate and sensitive, which can be used to determine the content of 8 kinds of fungal toxins in rice noodles.