免疫亲和净化-超高效液相色谱-串联质谱法测定食品中玉米赤霉烯酮类真菌毒素

建立食品中6种玉米赤霉烯酮类(α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮、玉米赤霉烯酮)真菌毒素的免疫亲和净化-超高效液相色谱-串联质谱检测的实验方法。样品经80%乙腈溶液提取,通过免疫亲和柱净化富集,用2 mL乙腈洗脱,氮吹至近干,0.5 mL 50%乙腈溶液复溶,采用超高效液相色谱-串联质谱进行测定。在ACQUITY UPLC HSS T3反相柱上分离,梯度洗脱,流动相为乙腈和水,质谱采集模式为电喷雾负离子多反应监测模式。6种目标物的线性范围为0.1~100μg/L,相关系数(R~2)均大于0.992,检出限为0.05μg/kg,定量限为0.2μg/kg,3个不同水平的加标平均回收率为73.0%~119.1%,相对标准偏差不大于10%。该方法具有操作简单、重复性好、灵敏度高、杂质干扰小等特点,可以用于食品中玉米赤霉烯酮类真菌毒素的检测。

Determination of Zeranols in Food by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Immunoaffinity Column Clean-up

A method was established for the determination of 6 zeranols (α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalanone, and zearalenon) in foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with immunoaffinity column clean-up. Sample extraction was carried out with 80% (V/V) acetonitrile-water mixture followed by purification on an immunoaffinity column, which was eluted with 2 mL of acetonitrile, and the eluate was blown to dryness by nitrogen and redissolved with 0.5 mL of 50% (V/V) acetonitrile-water mixture. The target compounds were assayed by UPLC-MS/MS. The chromatographic separation was performed on an ACQUITY UPLC HSS T3 column by gradient elution using acetonitrile and water as mobile phase. The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring (MRM) in the electrospray negative ionization mode. Good linearities (R2 > 0.992) were achieved for these 6 compounds over the concentration range of 0.1–100 μg/L. The limit of detection (LOD) of the method was 0.05 μg/kg, and the limit of quantification (LOQ) was 0.2 μg/kg. The mean recoveries of the 6 target compounds (spiked at three concentration levels) ranged from 73.0% to 119.1%, with relative standard deviations (RSDs) of not more than 10%. This method is suitable for the simultaneous determination of multiple zearalenonic mycotoxins in foods with simple pretreatment, high sensitivity, and good recovery.