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

中文关键词:  高效液相色谱-串联质谱  腐乳  真菌毒素  快速检测  QuEChERS

英文关键词:high performance liquid chromatography-tandem mass spectrometry  sufu  mycotoxin  rapid detection  QuEChERS

中文摘要:

      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0.22 μm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, 3 μm)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(electrospray ionization, 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。

英文摘要:

      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 0.22 μm polytetrafluoroethylene (PTFE) ultrafiltrate membrane, and then separated by Atlantis? T3 ultra high performance liquid chromatography column (2.1 mm×150 mm, 3 μm) 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.