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为保证中药三七质量和安全性,本文建立了一种同时检测三七药材中10种真菌毒素的超高效液相色谱串联质谱定量分析方法。三七药材以乙腈超声提取,多功能净化柱(HLB柱)净化,Phenomenex Kinetex XB-C18柱分离,用甲醇和含5 mmol·L-1醋酸铵水溶液为流动相进行梯度洗脱,以电喷雾离子源正负离子模式多反应监测方式检测。结果表明,10种毒素在各自线性范围内线性关系良好,相关系数r在0.998 1~1.000 0之间,定量限为0.15~8.6μg·kg-1,加标回收率为73.8%~107.0%,相对标准偏差为0.10%~10.9%。该方法净化效果好、灵敏度高、重复性好,适用于基质成分复杂的三七药材中多种真菌毒素的定量检测。
In order to ensure the quality and safety of Panax notoginseng, we established a method for the simultaneous determination of 10 mycotoxins in Panax notoginseng by ultra performance liquid chromatography-tandem mass spectrometry. Panax notoginseng was extracted with acetonitrile and purified by HLB column. Phenomenex Kinetex XB-C18 column was used for separation. The mobile phase was eluted with methanol and 5 mmol·L-1 ammonium acetate as eluent Ion source positive and negative ion mode multi-reaction monitoring method. The results showed that the ten toxins had a good linearity in the linear range of 0.998 1 ~ 1.000, the limit of quantification was 0.15 ~ 8.6 μg · kg-1, the recoveries were 73.8% -107.0% The relative standard deviation was 0.10% ~ 10.9%. The method has the advantages of good purification effect, high sensitivity and good repeatability, and is suitable for the quantitative detection of various mycotoxins in the Panax notoginseng medicinal materials with complex matrix components.