液相色谱法和液质联用法检测玉米中的脱氧雪腐镰刀菌烯醇的比较

Comparison of two detection methods of HPLC and LC-MS for the deoxynivalenol in corn

为了选择实验室准确检测脱氧雪腐镰刀菌烯醇的快速经济的方法,比较免疫亲和柱-高效液相色谱(HPLC)法和免疫亲和柱-液质联用(LC-MS)法检测脱氧雪腐镰刀菌烯醇。结果表明,两种方法的线性关系均良好,R^2=0.999 9;HPLC法、LC-MS外标法及内标法精密度试验结果相对标准偏差(RSD)分别为1.31%、1.20%及0.37%,回收率分别在80.77%～91.92%、108.71%～105.56%及113.48%～119.27%,精密度、回收率及重复性试验结果RSD均<5%;HPLC法的定量限和检出限分别为76.82μg/kg、23.05μg/kg,LC-MS法的定量限和检出限分别为1.67μg/kg、0.502μg/kg,均低于国标给定标准。LC-MS法灵敏度高,检出限低,但在检测由本底样品时,容易造成假阳性,HPLC法的提取溶剂是水,LC-MS法提取溶剂是乙腈。综合分析,在均能满足实验要求情况下,HPLC法更简便、经济、环保,可作为实验室大批量检测的首选。

In order to select a rapid and economical method for the accurate detection of deoxynivalenol in laboratory,the deoxynivalenol was determined by immunoaffinity column HPLC and immunoaffinity column LC-MS.The results showed that the linear relationship of the two methods were both good,R2=0.999 9.The relative standard deviations(RSD)of the precision tests results of HPLC method,external standard method and internal standard method of LC-MS were 1.31%,1.20%and 0.37%,respectively,the recovering rates were 80.77%-91.92%,108.71%-105.56%,and 113.48%-119.27%,respectively.The RSD of precision,recovering rate and repeatability tests results were all less than 5%.The quantitative limit and detection limit of HPLC method were 76.82μg/kg and 23.05μg/kg,respectively.The quantitative limit and detection limit of LC-MS method were 1.67μg/kg and 0.502μg/kg,respectively,which were lower than the national standard.But the sensitivity of LC-MS was high and the detection limit was low.It was easy to cause false positive in the detection of background samples,the extraction solvent of HPLC was water,and the extraction solvent of LC-MS was acetonitrile.As comprehensive analysis,under the condition that all could meet the experimental requirements,HPLC method was more convenient,economic and environmentally friendly,and was the first choice for large-scale laboratory detection.