凝胶渗透净化–超高效液相色谱–串联质谱法测定橙汁中链格孢霉毒素

Determination of Alternaria Toxins Residues in Orange Juice by UPLC–MS–MS Coupled with Gel Permeation Chromatography Purification

建立橙汁中4种链格孢霉毒素含量测定的凝胶渗透–超高效液相色谱–串联质谱检测方法。样品用乙腈提取后,用填料为Bio-Beads-S–X3的凝胶渗透色谱柱净化,净化时流动相采用乙酸乙酯–环己烷(体积比为1∶1),流速为5 mL/min,测定时用超高效液相反相C18色谱柱分离,甲醇–水系统梯度洗脱,采用电喷雾负离子源和多反应监测(MRM)模式定性和定量。4种链格孢霉毒素的最低定量限在0.0004～0.002 mg/kg范围内,加标回收率为78.9%～111.5%,测定结果的相对标准偏差均低于9.0%(n=10)。

A new method using gel permeation chromatography（GPC） clean up followed by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS-MS） was developed for the determination of 4 alternaria toxins in orange juice. Samples were extracted with acetonitrile, then purified by Bio-Beads-S-X3 GPC column with ethylacetate-cyclohexane（volume ratio was 1 ： 1） as the mobile phase at a flow rate of 5 mL/min. The chromatographic analysis was performed on an UPLC reversed-phase C18 column using methanol-water as a gradient solvent system. The qualitative and quantitative analysis were performed with negative ions electrospray ionization source and multiple reaction monitoring（MRM） mode. The quantitation limits of the four alternaria toxins were between 0.0004 mg/kg and 0.002 mg/kg. The recoveries ranged from 78.9% to 111.5% with relative standard deviations less than 9.0%（n=10）.