固相萃取柱净化-高效液相色谱法测定谷物中的呕吐毒素残留量

Determination of deoxynivalenol residues in cereal grains by solid phase extraction column clean-up coupled with high performance liquid chromatography

中文关键词:  固相萃取柱  高效液相色谱法  谷物  呕吐毒素

英文关键词:solid phase extraction column  high performance liquid chromatography  cereal grains  deoxynivalenol

中文摘要:

      目的 建立固相萃取柱净化-高效液相色谱法快速检测小麦、大麦、玉米及大米等谷物中呕吐毒素的残留量。方法 样品经乙腈-水提取液(85:15, V:V)提取, 过HLB固相萃取柱净化。采用C18柱为分离柱, 对流动相的组成和洗脱方式等参数进行优化和探讨。以水和甲醇为流动相进行梯度洗脱, 流速为0.8 mL/min, 柱温35 ℃, 外标法定量。结果 呕吐毒素浓度在0.05～5.0 mg/L的范围内线性关系良好, 相关系数均大于0.9999。呕吐毒素在0.5、1.0和2.0 mg/L添加水平的回收率为79.7%～106.0%, 相对标准偏差(relative standard deviation, RSD)小于4.2% (n=5), 方法定量限为300 μg/kg。结论 该方法简便、快捷、准确、灵敏度较高, 适用于小麦、大麦、玉米及大米等的谷物中呕吐毒素的快速检测。

英文摘要:

      Objective To establish the method for determination of deoxynivalenol residues in cereals such as wheat, barley, corn and rice by solid phase extraction column clean-up coupled with high performance liquid chromatography. Methods The sample was extracted with acetonitrile-water extract (85:15, V:V) and purified by HLB solid phase extraction column. The C18 column was used as the separation column to optimize and discuss the parameters such as the composition and elution mode of the mobile phase. Gradient elution was performed with water and methanol as mobile phases. The temperature of column was 35 ℃, the flow rate was 0.8 mL/min, then the sample was quantified by external standard method. Results The deoxynivalenol had a good linear relation in the concentration range of 0.05-5.0 mg/L, and the correlation coefficient was greater than 0.9999. The recoveries were ranged from 79.7% to 106.0% for the deoxynivalenol residues with 3 spiked levels of 0.5, 1.0 and 2.0 mg/L. The relative standard deviations (RSDs) were less than 4.2% (n=5), and the limits of quantitation (LOQ) for deoxynivalenol were 300 μg/kg. Conclusion This method is simple, rapid, accurate and sensitive, and is suitable for the rapid detection of deoxynivalenol in wheat, barley, corn and rice.