火腿中14种真菌毒素含量的QuEchERs提取-超高效液相色谱串联四级杆质谱测定法

Determination of 14 mycotoxins in hams with QuEchER based extraction and liquid chromatography tandem mass spectrometry

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B_(1)、伏马毒素B_(2)、伏马毒素B_(3)、黄曲霉毒素B_(1)、黄曲霉毒素B_(2)、环匹阿尼酸、黄曲霉毒素G_(1)、黄曲霉毒素G_(2)、橘青霉素、蛇形菌素、T_(2)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20 mL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0.5~100μg/L之间,相关系数均>0.997,定量下限为1.67~66.67μg/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。

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 B_(1),fumarins B_(2),fumarins B_(3),aflatoxin B_(1),aflatoxin B_(2),cyclopianic acid,aflatoxin G_(1),aflatoxin G_(2),citronillin,ophiformin,T_(2) 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 100μg/L,with correlation coefficients>0.997.The lower limit of quantification(L0Q)were 1.67 to 66.67μg/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.