液质联用法筛查药食同源中药中多种真菌毒素

Screening of Mycotoxins in Traditional Chinese Medicine and Food by LC-MS/MS

建立药食同源中药材中13种真菌毒素的超高效液相色谱-四极杆串联离子阱复合质谱法测定方法。样品经乙腈-甲醇-甲酸-水(60︰20︰1︰19,V/V)提取,QuEChERS方法净化,C_(18)色谱柱分离,流动相为乙腈和0.1%甲酸水溶液,梯度洗脱,电喷雾正离子模式电离,MRM-IDA-EPI扫描模式检测,外标法定量。结果表明,13种真菌毒素在0.05~20 ng/mL范围内均呈现良好线性关系,相关系数(r)均大于0.993。平均加标回收率为66.3%~91.8%,相对标准偏差为2.8%~7.7%,方法检出限为0.1~0.8μg/kg。该方法应用超高效液相色谱-四极杆串联离子阱复合质谱特有的多反应监测-信息关联扫描-增强子离子扫描(MRM-IDA-EPI)扫描模式,可同时实现化合物的准确定性、定量分析及可疑峰筛查、确证。

A method for the determination of thirteen mycotoxins in medicinal and edible homologous Chinese medicinal materials by ultra-high performance liquid chromatography quadrupole tandem ion trap composite mass spectrometry was established.The samples were extracted with acetonitrile and methanol and formic acid and water(60︰20︰1︰19,V/V),purified by QuEChERS method,separated with C_(18)chromatographic column for gradient elution using acetonitrile and 0.1%formic acid aqueous solution as mobile phase,ionized by electrospray positive ion mode,detected by MRM-IDA-EPI scanning mode,and quantified by external standard method.The results showed that a total of 13 mycotoxins had good linear relationships in the range of 0.05-20 ng/mL,and the correlation coefficients were larger than 0.993.The limits of detection were 0.1-0.8μg/kg.The average standard recoveries of apple puree were 66.3%-91.8%,and the relative standard deviations were 2.8%-7.7%.The MRM-IDA-EPI scanning mode of ultra-performance liquid chromatography quadrupole tandem ion trap composite mass spectrometry was used to realize the accurate qualitative and quantitative analysis of compounds and the screening and confirmation of suspicious peaks.