摘要
目的 建立QuEchERs提取-超高效液相色谱法串联三重四级杆质谱法测定火腿中14种真菌毒素(伏马毒素B1、伏马毒素B2、伏马毒素B3、黄曲霉毒素B1、黄曲霉毒素B2、环匹阿尼酸、黄曲霉毒素G1、黄曲霉毒素G2、橘青霉素、蛇形菌素、T2毒素、新茄镰孢菌醇、杂色曲霉素、赭曲霉毒素A)的方法.方法 用20mL乙腈+水+甲酸(80+19+1)提取火腿样品,提取液经QuEchERs净化,以0.1％甲酸水和乙腈为流动相,待测液经C18色谱柱分离,多重反应监测模式定量检测.结果 经过测试,14种真菌的毒素含量在0.5～100 μg/L之间,相关系数均＞0.997,定量下限为1.67～66.67 µg/kg.此外,加标回收率为79.1％～96.2％,且相对标准偏差为1.1％～9.5％.结论 所建立的QuEchERs提取-超高效液相色谱串联四级杆质谱检测方法快速、准确、灵敏,适用于火腿中14种真菌毒素的检测.
Abstract
Objective To establish a QuEchERs extraction and ultra high performance liquid chromatography tandem triple quadrupole mass spectrometry(LC-MS/MS)method for the determination of 14 mycotoxins(fumarins B1,fumarins B2,fumarins B3,aflatoxin B1,aflatoxin B2,cyclopianic acid,aflatoxin G1,aflatoxin G2,citronillin,ophiformin,T2 toxin,Neosolanol,Sterigmatocystin,and Ochratoxin A)in hams.Methods The ham samples were extracted by 20 mL 80％acetonitrile(acetonitrile+water+formic acid=80+19+1).The extracts were purified by QuEchERs,and the mobile phases were 0.1％formic acid water and acetonitrile.The samples were separated by C18 column and quantitated by multiple reaction monitoring(MRM).Results After testing,the toxin content of 14 mycotoxins ranged from 0.5 to 100 μg/L,with correlation coefficients＞0.997.The lower limit of quantification(LOQ)were 1.67 to 66.67 μg/kg.In addition,the spiked recoveries was 79.1％-96.2％,and the relative standard deviation were 1.1％-9.5％.Conclusion The QuEchERs extraction ultra-high performance liquid chromatography tandem quadrupole mass spectrometry detection method established is fast,accurate,sensitive,and suitable for the detection of 14 mycotoxins in ham.
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