高效液相色谱-串联质谱法测定稻谷和糙米中的溴硝醇

Determination of 2-bromo-2-nitropropane-1,3-diol residues in grain and unpolished rice by high performance liquid chromatography-tandem mass spectrometry

建立了稻谷和糙米中溴硝醇的高效液相色谱-串联质谱检测方法。样品采用酸性乙腈提取,经HLB固相萃取柱净化,以Hypersil GOLD-C_(18)柱分离,在负离子模式下采集数据,基质外标法定量。溴硝醇在电喷雾负离子模式下的母离子m/z 167.8,实际为溴硝醇发生反应后的产物2-溴-2-硝基乙醇的分子离子峰。溴硝醇在0~5.0μg/mL浓度范围内呈良好线性,线性相关系数大于0.99,平均回收率为86.2%~94.6%,相对标准偏差不超过13%。该方法适用于大批量粮谷样品中溴硝醇的快速检测。

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 2-bromo-2-nitropropane-1,3-diol residues in grain and unpolished rice products.The acetonitrile solution containing formic acid and HLB solid phase extraction column were used for the extraction and purification of 2-bromo-2-nitropropane-1,3-diol,respectively,following separation via Hypersil GOLD-C_(18)column.The target analyte was detected in the negative ion mode using an electrospray ionization(ESI)source with external standard method.The parent ion m/z 167.8 of 2-bromo-2-nitropropane-1,3-diol was actually the molecular ion peak of 2-bromo-2-nitroethanol,which was the degraded product of reversible aldehyde alcohol reaction of 2-bromo-2-nitropropane-1,3-diol.The results showed that there was a good relationship with correlation coefficient above 0.99 in the concentration range of 0-5.0μg/mL.Average recoveries for the residues were in the range of 86.2%to 94.6%,and the relative standard deviations(RSDs)was no more than 13%in grain and unpolished rice products.The developed method was suitable to determinate 2-bromo-2-nitropropane-1,3-diol residues in grain and unpolished rice.