高效液相色谱-串联质谱法测定腐乳中16种真菌毒素

Determination of 16 mycotoxins in sufu by high performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱法快速筛查和定量测定腐乳中16种真菌毒素的方法.方法腐乳样品用QuEChERS方法提取,经Oasis PRiME HLB小柱净化后,用0.22μm聚四氟乙烯(polytetrafluoroethylene,PTFE)滤膜滤过,滤液采用Atlantis■T3超高效液相色谱柱(2.1 mm×150 mm,3μm)分析,以0.1%甲酸水溶液(A)~0.1%甲酸乙腈(B)作为流动相体系,进行梯度洗脱分离,在电喷雾(electrosprayionization,ESI)正负离子扫描模式下,以多反应监测(multiple reaction monitoring,MRM)为基础,高效液相色谱-串联质谱法对16种真菌毒素进行定量测定.结果16种真菌毒素在各自的浓度范围内,线性相关性良好,相关系数(r)均大于0.996,在高、中、低3个回收水平的回收率为71.34%~117.60%,相对标准偏差(relative standard deviation,RSD)处于0.46%~8.31%之间(n=6).结论本方法灵敏度高,再现性好,适用于腐乳中黄曲霉毒素、伏马毒素、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、桔青霉素等16种真菌毒素的快速筛查与定量检测.

Objective To establish a method for rapid screening and quantitative determination of 16 mycotoxins in sufu by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods Sufu were extracted by QuEChERS method,purified by the Oasis PRiME HLB column,filtrated by 0.22μm polytetrafluoroethylene(PTFE)ultrafiltrate membrane,and then separated by Atlantis■T3 ultra high performance liquid chromatography column(2.1 mm×150 mm,3μm)with a gradient elution of 0.1%formic acid(mobile phase A)-0.1%formic acid acetonitrile(mobile phase B)in electrospray(ESI)ion scanning mode,based on the multiple reaction monitoring(MRM).The quantitative determination of 16 kinds of mycotoxins was carried out by HPLC-MS/MS.Results The 16 kinds of mycotoxins had good linear relationships in the certain concentrate,with the correlation coefficients(r)all over 0.996.The recoveries at the high,medium and low levels were 71.34%-117.60%,and the relative standard deviations(RSDs)were 0.46%-8.31%(n=6).Conclusion This method has high sensitivity and good reproducibility,which is suitable for the rapid screening and quantitative detection of 16 mycotoxins such as aflatoxin,fumonisin,zearalenone,deoxynivalenol,and citrinin in sufu.