葡萄酒中恶霜灵残留液相色谱-串联质谱检测

目的]建立了葡萄酒中中恶霜灵残留量的液相色谱-串联质谱分析方法。方法]样品直接注入液相色谱仪,经AgilentXDB-C18色谱柱分离,以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱。以电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测,基质匹配标准溶液外标法定量。结果]恶霜灵2-400μg/L范围内呈线性相关,相关系数（r）均大于0.999;其定量限为5μg/L。葡萄酒样品在5、10和20μg/L添加水平时,恶霜灵的回收率范围分别为91.5%-111.2%,相对标准偏差（RSD）分别为6.2%-8.6%,可以满足葡萄酒中恶霜灵残留量的检测需要。结论]本方法无需前处理,灵敏度高,选择性好,同时定性定量,对葡萄酒中恶霜灵含量的测定及评估更为准确。

Determination of Oxadixyl Residue in Wines by Liquid Chromatography-Tandem Mass Spectrometry Method

A liquid chromatography-tandam mass spectrometric（LC-MS/MS） method was developed for determination of oxadixyl residue in wines.The test sample was injected directly.The separation was performed on a Agilent XDB-C18 column by using the gradient elution with 0.1% formic acid solution and acetonitrile.The residue was determined by electrospry ionization-tandem mass spectrometry,quantified by matrix-matched external standard method.The calibration curves shown good linearity in the 2-400 μg/L levels with the correlation coefficients r0.999.The limit of quantitative was 5 μg/L.The recoveries of oxadixyl in wines at 5,10 and 20 μg/L were in the range of 91.5%-111.2%.The relative standard deviations were 6.2%-8.6%.The method can meet the requirements for determination of oxadixyl residue in wines for import and export inspection.