QuEChERS-超高效液相色谱-串联三重四级杆质谱法同时测定玉米秸秆饲料中20种真菌毒素

Simultaneous determination of 20 kinds of mycotoxins in maize straw feed by QuEChERS-ultra performance liquid chromatography-triple quadrupole mass spectrometry

试验旨在建立QuEChERS-超高效液相色谱-串联三重四级杆质谱法(UPLC-MS/MS)同时测定玉米秸秆饲料中20种真菌毒素含量的方法。样品经乙腈-甲酸(95∶5)混合溶液超声提取后,加入无水硫酸镁、N-丙基乙二胺(PSA)、十八烷基键合硅胶吸附剂(C18)净化,取适量上清液氮气吹至近干,使用甲醇-水-甲酸(30∶70∶0.1)混合溶液复溶,过PTFE滤膜,采用C18色谱柱分离,多反应监测模式(MRM)检测,外标法进行结果定量。结果显示,20种真菌毒素线性关系良好,相关系数(R2)均大于0.99,检出限和定量限范围分别为0.15~3.10μg/kg和0.49~10.33μg/kg,在低、中、高3个不同水平下的加标回收率范围为70.4%~118.3%,相对标准偏差范围为1%~10%(n=6)。研究表明,试验方法操作简单、重现性好,灵敏度和准确度高,可用于玉米秸秆饲料中真菌毒素的日常筛查工作。

The experiment was to establish an analytical method for the simultaneous determination of 20 kinds of mycotoxins in maize straw feed by QuEChERS-UPLC-MS/MS.The samples were extracted with acetonitrile-acetic acid(95∶5),and the supernatant was purified by anhydrous MgSO4,PSA and C18.Then an appropriate amount of supernatant was blown to dry with nitrogen.The samples were reconstituted with methanol-water-acetic acid(30∶70∶0.1),passed through a PTFE filter membrane,and separated on a C18 chromatographic column.Using the multiple reaction monitoring(MRM)scan mode to monitor the target compounds and the results were quantified by the external standard method.The results showed that the linear ranges of the 20 mycotoxins were good,and the correlation coefficients(R^(2))were greater than 0.99.The limits of detection were 0.15~3.10μg/kg,with limits of quantification were 0.49~10.33μg/kg.The recoveries at the three levels were within the range of 70.4%~118.3%,with relative standard deviations of 1%~10%(n=6).The study indicates that the method was easy to operate,reproducible and highly accurated and sensitive,which can be used for routine screening of mycotoxins in corn stalk feed.