UPLC-ESI-MS-MS结合QuEChERS同时测定柑橘中的4 种真菌毒素

建立同时检测柑橘中链格孢酚甲基乙醚、交链孢酚、腾毒素和橘青霉素4 种真菌毒素的QuEChERS-超高效液相色谱-质谱分析方法。待测样品经乙腈提取，无水MgSO4和NaCl脱水盐析，C18键合相分散萃取净化，以ACQUITY UPLC BEH C18液相色谱柱为分离柱，以0.1%甲酸溶液和乙腈作为流动相梯度洗脱，在电喷雾离子源电离、多反应监测模式条件下进行测定，外标法定量。该方法在5.0～200 μg/L范围内线性关系良好，相关系数（R2）不小于0.992 7，检出限为0.2～0.7 μg/kg。3 个不同加标水平的平均回收率为78.0%～103.3%，相对标准偏差为2.6%～10.6%。结果表明，该方法快速、准确、灵敏，适用于柑橘中4 种真菌毒素残留的快速确证检测。

Simultaneous Determination of Four Mycotoxins in Citrus Fruits by Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry Combined with Modified QuEChERS

A method was developed for simultaneous determination of four mycotoxins (aletrnariol monomethyl ether,
tentoxin, alternariol, and citrinin) in citrus fruits using ultra-performance liquid chromatography-tandem mass spectrometry
combined with optimized QuEChERS. Samples were extracted with acetonitrile, salted out with anhydrous MgSO4 and
NaCl, cleaned up with C18 and then analyzed using UPLC-MS-MS in multiple reaction monitoring (MRM) mode with
electrospray ionization. The separation of the target mycotoxins was performed on an ACQUITY UPLC BEH C18 liquid
chromatography column through gradient elution using a mobile phase consisting of acetonitrile and 0.1% formic acid
aqueous solution and the matrix-matched external standard calibration was used for quantitation. This method had a good
linearity in the concentration range of 5.0–200 μg/L with correlation coefficients (R2) more than 0.992 7, and the limit of
detection of the established method was in the range of 0.2–0.7 μg/kg. The average recoveries of the four mycotoxins in
different matrixes (citrus pulp, peel and whole fruit) at three spiked levels ranged from 78.0% to 103.3%, with relative
standard deviations (RSDs) of 2.6%–10.6%. This method is simple, quick, accurate, sensitive, and suitable for the quick
confirmation and quantitative determination of the four mycotoxins in citrus fruits.