不同前处理方法对山药中13种真菌毒素检测的影响

Effects of Different Pretreatment Methods on the Detection of 13 Mycotoxins in Yam

通过优化前处理步骤,建立简单、高效、无须净化并能同时检测13种真菌毒素的超高效液相色谱-串联质谱方法。样品经过甲醇/水(80/20,V/V)-0.1%甲酸、乙腈/水(80/20,V/V)-0.1%甲酸,二次超声提取,氮吹浓缩,采用超高效液相色谱-串联质谱仪测定。用基质配制标准曲线,外标法进行定量分析。结果表明,相关系数均大于0.997,在低、中、高3个加标浓度,回收率为69.3%~112.4%,相对偏差为0.6%~7.4%。线性范围、准确度、精密度均符合要求,能快速高效检测山药中13种毒素。

By optimizing the pretreatment steps,a simple and effective UPLC-MS/MS method was established,which need not purification and can simultaneously detect 13 mycotoxins.The samples were extracted with methanol/water(80/20,V/V)-0.1%formic acid and acetonitrile/water(80/20,V/V)-0.1%formic acid successively.The extraction solution was combined,concentrated to constant volume by nitrogen blown concentration and then detected by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The standard curve prepared by matrix was used for qualitative and quantitative analysis with external standard method of quantitation.The correlation coefficients of 13 different mycotoxins were all greater than 0.997.The recoveries ranged from 69.3%~112.4%,with relative deviations of 0.6%~7.4%.The linear range,accuracy and precision all meet the requirements.The method was quickly detected 13 mycotoxins in yam.