建立了高效液相色谱-线性离子阱高分辨质谱（ HPLC-LTQ／Orbitrap MS）鉴定稻曲球中5种稻曲病菌毒素的方法。样品匀浆后以水为提取剂超声提取10 min，混合阳离子交换柱 PCX净化，采用 Xselect HSS T3色谱柱（150 mm×2.1 mm，3.5μm）分离，以水（含0.1％（v／v）甲酸）和甲醇为流动相，梯度洗脱。在m／z 200~1000范围内进行一级质谱全扫描，结合准分子离子峰的精确质量数和同位素相对丰度进行质谱分析。结果表明，鉴定到5种稻曲病菌毒素，质量准确度小于1×10－6（1 ppm），同位素相对丰度偏差绝对值≤3.3％，二级质谱碎片离子与理论裂解一致，回收率为90％~105％。该方法简便，灵敏度高，定性准确，为稻曲病菌产毒能力等相关研究提供了技术手段。
A sensitive method was developed for the simultaneous identification of five ustilox-ins 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×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 1×10-6(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 theoreti-cal 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.
参考文献
| [1] | Varga, E.;Glauner, T.;Berthiller, F.;Krska, R.;Schuhmacher, R.;Sulyok, M..Development and validation of a (semi-)quantitative UHPLC-MS/MS method for the determination of 191 mycotoxins and other fungal metabolites in almonds, hazelnuts, peanuts and pistachios[J].Analytical and bioanalytical chemistry,201315(15):5087-5104. |
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