首页|高通量高效快速净化方法结合UPLC-MS/MS测定粮食中黄曲霉毒素

高通量高效快速净化方法结合UPLC-MS/MS测定粮食中黄曲霉毒素

扫码查看
建立粮食中黄曲霉毒素B1、B2、G1、G2快捷高效的确证检测方法.通过对色谱及质谱分析条件、震荡提取方式、稀释倍数分别优化确定满足黄曲霉毒素B1、B2、G1、G2检测方法的最优条件,同时,开发一款自动过柱仪与快速净化柱配合使用对粮食中杂质进行高通量的高效净化,并采用超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测分析.粮食样品经 84%乙腈水溶液提取、Speedy Prep®-Myco1流穿式净化柱净化,使用ACQUITY UPLC BEH C18 色谱柱分离,以 0.1%甲酸水和乙腈作为流动相进行梯度洗脱,质谱采用电喷雾正离子模式和多反应监测模式(multiple reaction monitoring,MRM)采集信号,外标法定量.对于大米、小黄米、小麦、黄豆、面粉、大麦、黑米、花生、玉米基质,本方法黄曲霉毒素B1、B2、G1、G2的检出限和定量限分别为 0.06~0.12 μg/kg和 0.20~0.40 μg/kg,在其线性范围内相关系数R≥0.9993,在 0.2、0.4、1、10、20、40 μg/kg添加回收率为 72.37%~118.4%,相对标准偏差(RSD,n=6)为 0.64%~14%,回收率和精密度良好.该方法前处理操作简单、稳定性好,适用于粮食中黄曲霉毒素B1、B2、G1、G2的检测.
Determination of aflatoxins in grains using the high-throughput high efficient clean-up method and ultra-high performance liquid chromatography-tandem mass spectrometry
A simple and efficient method for determination of aflatoxins B1,B2,G1 and G2 in grains was established.By optimizing the chromatographic and mass spectrometry analysis conditions,oscillation extraction mode and dilution ratio,the optimal conditions satisfying the detection methods of aflatoxin B1,B2,G1 and G2 were determined respectively.At the same time,an high-throughput automatic presser was developed and used in combination with the flow-through clean-up column for high-throughput and efficient purification of impurities in grain.Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used for detection and analysis.The grinded grain sample was extracted by 84%acetonitrile solution and purified by Speedy Prep®-Myco 1 clean-up column.During UPLC-MS/MS quantification through external standard method,the purified extract was gradient eluted by ACQUITY UPLC BEH C18 column with 0.1%formic acid solution in water and acetonitrile as the mobile phase.Mass spectrometric signal collection was performed by electrospray positive ion and multiple reaction monitoring(MRM)mode.For rice,small yellow rice,wheat,yellow bean,flour,barley,black rice,peanut and corn,the limits of detection(LODs)and the limits of quantification(LOQs)of aflatoxins B1,B2,G1 and G2 were 0.06-0.12 μg/kg and 0.20-0.40 μg/kg with correlation coefficients higher than 0.9993 in their linear ranges.At spiked levels of 0.2,0.4,1,10,20 and 40 μg/kg,aflatoxins B1,B2,G1 and G2 were obtained with recoveries between 72.37%to 118.4%and relative standard deviations(RSD,n=6)between 0.64%to 14%.The recoveries and precision were good.This method is simple and stable,and is suitable for the detection of aflatoxin B1,B2,G1 and G2 in grain.

aflatoxinultra-high performance liquid chromatography-tandem mass spectrometrygrainhigh-throughput automatic presserhigh efficient sample preperation

何洁、余婷婷、梁松、王冰、李鹏、殷果、王炳志、徐梅、马红圳、闫研、严义勇

展开 >

深圳市易瑞生物技术股份有限公司,广东深圳 518101

深圳职业技术大学集成电路关键材料研究院,广东深圳 518055

深圳药品检验研究院,广东深圳 518055

澳门大学中华医药研究院中药质量研究国家重点实验室,澳门 999078

展开 >

黄曲霉毒素 超高效液相色谱-串联质谱 粮食 高通量自动过柱仪 高效前处理

广东省粤港湾联合创新领域项目深圳市技术攻关重点项目

2021A0505080003JSGG20191115141601721

2024

中国测试
中国测试技术研究院

中国测试

CSTPCD北大核心
影响因子:0.446
ISSN:1674-5124
年,卷(期):2024.50(5)