CAJ | 학술논문

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。
건립료고효액상색보-선성리자정고분변질보（ HPLC-LTQ／Orbitrap MS）감정도곡구중5충도곡병균독소적방법。양품균장후이수위제취제초성제취10 min，혼합양리자교환주 PCX정화，채용 Xselect HSS T3색보주（150 mm×2.1 mm，3.5μm）분리，이수（함0.1％（v／v）갑산）화갑순위류동상，제도세탈。재m／z 200~1000범위내진행일급질보전소묘，결합준분자리자봉적정학질량수화동위소상대봉도진행질보분석。결과표명，감정도5충도곡병균독소，질량준학도소우1×10－6（1 ppm），동위소상대봉도편차절대치≤3.3％，이급질보쇄편리자여이론렬해일치，회수솔위90％~105％。해방법간편，령민도고，정성준학，위도곡병균산독능력등상관연구제공료기술수단。
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.