Oasis HLB固相萃取-超快速液相-三重四极杆质谱法测定花生和花生油中黄曲霉毒素B1、B2、G1、G2

Determination of aflatoxin B1,B2,G1,G2in peanut and peanut oil using oasis HLB SPE-Ultra fast liquid chromatography-triple quadrupole tandem mass spectrometry

目的建立了Oasis HLB固相萃取-超快速液相-三重四极杆质谱法测定花生和花生油中黄曲霉毒素B1、B2、G1、G2的方法。方法样品用甲醇-水（V甲醇∶V水=20∶80）提取,离心后过Oasis HLB柱萃取净化,超快速液相进行梯度洗脱,质谱用电喷雾离子源（ESI）,经过正离子MRM模式,外标法定量。结果黄曲霉毒素（AFT）B1、B2、G1、G2的最低检出限分别为：0.05、0.05、0.10、0.20μg/kg,平均加标回收率在89.3%-98.7%之间,精密度（RSD）在2.6%-5.3%之间。结论本法利用Oasis HLB固相萃取柱良好的性能和质谱仪采用弯曲180度的碰撞池技术大大减少了样品中的杂质干扰,精密度和准确度高,方法操作简便,结果可靠。

Objective To establish a method to determine aflatoxin B1,B2,G1,G2 in peanut and peanut oil by oasis HLB SPE-high performance liquid chromatography-triple qua-drupole tandem mass.Methods The sample underwent methanol-water（V∶V=20∶80）extraction,and was then purified using oasis（R）HLB cartridge after centrifugation.Through gradient elution of liquid chromatography,ESI as mass spectrum,and positive ion MRM mode,the sample was quantified using external standard method.Results The minimum detection limit for AFT B1,B2,G1 and G2 were 0.05,0.05,0.10 and 0.20 ng/kg respectively while the average recovery rate of standard addition was 89.3%-98.7% and RSD was 2.6%-5.3%.Conclusions By optimizing sample extraction conditions,methods of precise extractions of oasis HLB SPE and cell collision of mass spectrometry bending with 180 degree were adopted to reduce the amount of disturbing impurities in the samples and to increase precision and accuracy.This method can be easily applied while the results are reliable.