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探讨固相萃取方法,超高效液相色谱串联质谱仪(UPLC-MS/MS)测定麦芯粉中4种交链孢毒素。样品经0.05 mol/L Na H2PO4(pH 3.0)-乙腈-甲醇超声提取(450+450+100,V/V),上清液过HLB固相萃取柱净化,以1.0 mmol/L氨水溶液(pH 8.3)-甲醇为流动相,经Waters CORTECS C18(4.6×100 mm,2.7μm)柱分离梯度洗脱,采用电喷雾负离子(ESI-)、多反应监测(MRM)模式检测;以基质加标工作曲线定量。细交链孢菌酮酸(TeA)、交链孢酚(AOH)在2.0μg/L~100μg/L浓度范围内,腾毒素(TEN)、交链孢酚单甲醚(AME)在0.2μg/L~10.0μg/L浓度范围内线性关系良好,相关系数(R2)均大于0.998。回收率为76.3%~107.5%,TeA、AOH检出限和定量限分别为1.0μg/kg和3.0μg/kg、TEN、AME检出限和定量限分别为0.1μg/kg和0.3μg/kg。该方法灵敏度高,简便,准确。适于测定麦芯粉中的交链孢毒素。
To study the solid-phase extraction and UPLC-MS / MS for the determination of four kinds of Alternaria toxin in wheat kernel powder. The samples were purified by ultrasonication (450 + 450 + 100, V / V) with 0.05 mol / L Na H2PO4 (pH 3.0) -acetonitrile-methanol and the supernatant was purified by HLB SPE. 8.3) -Methanol as the mobile phase and eluted with a Waters CORTECS C18 (4.6 × 100 mm, 2.7 μm) column with gradient elution by electrospray ionization (ESI-) and multi-reaction monitoring (MRM) Curve quantitative. In the concentration range of 2.0μg / L to 100μg / L, TEN and AME were incubated in the presence of 0.2μg of TeA and AEC. / L ~ 10.0μg / L concentration within a good linear relationship, the correlation coefficient (R2) is greater than 0.998. The detection limits and quantification limits of TeA and AOH were 1.0μg / kg and 3.0μg / kg, the detection limits and the limits of quantification of TEN and AME were 0.1μg / kg and 0.3μg / kg respectively . The method is sensitive, simple and accurate. It is suitable for the determination of Alternaria toxin in wheat flour.