[Identification of ustiloxins in false smut balls of rice based on high performance liquid chromatography-high...

A sensitive method was developed for the simultaneous identification of five ustiloxins in the false smut balls of rice by high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (HPLC-LTQ/Orbitrap MS). The samples were extracted with deionized water under ultrasonic condition for 10 min, then purified by a strong cation exchange column (PCX). The ustiloxins were separated on an Xselect HSS T3 column (150 mm x 2.1 mm, 3.5 μm) by using 0.1% (v/v) formic acid water solution and methanol as mobile phases with gradient elution at a flow rate of 0.3 mL/min. The full scan range was m/z 200-1 000. The confirmatory analysis of the target compounds was carried out by the accurate mass of quasi-molecular ion, isotope abundance ratio and qualitative fragments. The results showed that the five ustiloxins (A, B, C, D and F) were identified from the false smut balls with mass accuracy less than 1 x 10(-6) (1 ppm) and the absolute values of the deviation of isotope abundance ratio were not more than 3.3%. The product ions were consistent with the theoretical fragment mode. The recoveries were 90% to 105%. This method is accurate and sensitive for the simultaneous identification of the five ustiloxins, which can provide technical means for the research of the ability in toxin producing by Ustilaginodea virens.