基于复合萃取技术-超高效液相色谱-串联三重四极杆质谱法同时测定谷物及其制品中10种真菌毒素

Simultaneous determination of 10 kinds of mycotoxins in grain and grain products based on composite extraction technology coupled with ultra performance liquid chromatography-tandem with triple quadrupole mass spectrometry

中文关键词:  分散固相萃取  超高效液相色谱串联三重四极杆质谱法  真菌毒素  谷物

英文关键词:dispersed solid phase extraction  ultra performance liquid chromatography-tandem with triple quadrupole mass spectrometry  mycotoxins  grain

中文摘要:

      目的 建立超高效液相色谱-串联三重四极杆质谱法(ultra performance liquid chromatography-tandem with triple quadrupole mass spectrometry, UPLC-MS/MS)同时测定谷物及其制品中的10种真菌毒素的检测方法。方法 以0.1%甲酸-80%乙腈水为提取溶剂, 经过涡旋、振荡提取后, 加入Supel QuE z-sep+作为净化剂进行初级净化, 离心后的上清液过PRiME HLB固相萃取柱二次净化, 经UPLC-MS/MS测定, 质谱采用多反应监测模式定性, 基质匹配标准溶液外标法定量。结果 10种真菌毒素在谷物中的检出限为0.10~10.00 μg/kg, 定量限为0.35~20.00 μg/kg。在玉米、花生、大米3种谷物基质中的回收率为73.2%~98.1%, 相对标准偏差为1.3%~9.3%。结论 该方法的灵敏度满足国家标准对真菌毒素的限量要求, 实验操作简便快速, 成本较低, 定性定量分析可靠, 适合谷物中真菌毒素的多组分高通量快速分析测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 10 kinds of mycotoxins in grain and grain products based on composite extraction technology coupled with ultra performance liquid chromatography-tandem with triple quadrupole mass spectrometry (UPLC-MS/MS). Methods Using 0.1% formic acid-80% acetonitrile water as extraction solvent, after vortex and oscillation extraction, Supel QuE z-sep+ was added as purifying agent for primary purification, and the supernatant after centrifugation was purified by PRiME HLB solid phase extraction column for the second time, and was determined by UPLC-MS/MS. The mass spectrometry was characterized by multiple reaction monitoring mode and quantified by matrix matching standard solution external standard method. Results The limits of detection of 10 kinds of mycotoxins in cereals were 0.10?10.00 μg/kg, and the limits of quantitative were 0.35?20.00 μg/kg. The recoveries in corn, peanut and rice were 73.2%?98.1%, and the relative standard deviations were 1.3%?9.3%. Conclusion The sensitivity of this method meets the limit requirements of national standards for mycotoxins. The experimental operation is simple and rapid, the cost is low, the qualitative and quantitative analysis is reliable, and it is suitable for multi-component high-throughput rapid analysis and determination of mycotoxins in cereals.