超高效液相色谱-串联质谱法测定牛奶中24种真菌毒素

Determination of 24 Mycotoxins in Milk by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

运用基质分散固相萃取净化,建立牛奶中24种真菌毒素(黄曲霉毒素B_(1)、黄曲霉毒素B_(2)、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、赭曲霉毒素A、玉米赤霉烯酮、玉米赤霉酮、α-玉米赤霉烯醇、β-玉米赤霉烯醇、α-玉米赤霉醇、β-玉米赤霉醇、T-2毒素、HT-2霉素、伏马毒素B_(1)、伏马毒素B_(2)、伏马毒素B_(3)、脱氧雪腐镰刀菌烯醇、3-乙酰脱氧雪腐镰刀菌烯醇、15-乙酰脱氧雪腐镰刀菌烯醇、交链孢霉单甲基醚、交链孢酚、腾毒素、细交链孢菌酮酸)多残留检测的超高效液相色谱-串联质谱检测方法。样品经80%乙腈溶液(体积分数)提取,通过基质分散固相萃取净化,氮吹至近干,1 mL 50%乙腈溶液(体积分数)复溶,采用超高效液相色谱-串联质谱进行测定。经ACQUITY UPLC HSS T3反相柱(2.1 mm×100 mm,1.8μm)分离,梯度洗脱,采用电喷雾离子源-多反应监测模式采集。24种目标物的相关系数(R2)均大于0.985,加标回收率为71.0%~123.0%,相对标准偏差均小于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,可以用于牛奶中24种真菌毒素的检测。

A method was developed for the multi-residue determination of 24 mycotoxins including aflatoxin B_(1)(AFB_(1)),AFB_(2),AFG1,AFG2,AFM1,ochratoxin A(OTA),zearalanone,zearalenone,α-zearalanol,β-zearalanol,α-zearalenol,β-zearalenol,T-2 toxin,HT-2 toxin,fumonisin B_(1)(FB_(1)),FB_(2),FB_(3),deoxynivalenol(DON),3-DON,15-DON,alternariolmethylether,alternariol,tentoxin and tenuazonic acid in milk by ultra-high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS).The sample was extracted with 80% aqueous acetonitrile,the extract was purified by matrix solid-phase dispersion(MSPD) extraction and blown to dryness under nitrogen,and the residue was redissolved in 1 mL of 50% aqueous acetonitrile(V/V) and analyzed by UPLC-MS/MS.An acquity UPLC HSS T3(2.1 mm ×100 mm,1.8 μm) reversed-phase column was used for the separation with gradient elution.Detection was performed under the multiple reaction monitoring(MRM) mode using electrospray ionization.The correlation coefficients(R2) for all analytes were greater than 0.985,the recoveries for spiked samples ranged from 71.0% to 123.0%,and the relative standard deviation(RSD) was less than 10%.The developed method has the advantages of simple operation,good repeatability,high sensitivity and low impurity interference and can be used for the determination of the 24 mycotoxins in milk.