液质联用法测定食品中氯酸盐和高氯酸盐

Determination of Chlorate and Perchlorate in Food Coupled with High Liquid Chromatography-Tandem Mass Spectrometry

该试验旨在建立食品中氯酸盐和高氯酸盐残留的液相色谱-串联三重四极杆质谱联用测定方法。样品经70%乙腈水溶液超声提取,PRiME HLB固相萃取柱净化,以资生堂PC HILIC色谱柱(150 mm×2.0 mm,5μm)分离,负离子多反应监测模式监测,内标法定量。结果显示:氯酸盐和高氯酸盐在0.5~50μg/L范围内呈线性关系,相关系数分别为0.9992和0.9994。一般食品基质中氯酸盐定量限及检出限分别为2.0μg/kg和0.5μg/kg,高氯酸盐定量限及检出限分别为1.0μg/kg和0.5μg/kg。包装饮用水中氯酸盐定量限及检出限分别为0.25μg/kg和0.50μg/kg;高氯酸盐的定量限及检出限分别为0.25μg/kg和0.50μg/kg。当加标浓度分别为10,20和50μg/kg时,其平均方法回收率为80.1%~119.5%,平均相对标准偏差为2.1%~9.9%(n=6)。该方法适用于食品中氯酸盐和高氯酸盐的监测。

To establish a detection method for chlorate and perchlorate residues in food coupled with high liquid chromatography-tandem mass spectrometry,the analytes extracted and protein removed in samples were used by 70%acetonitrile water solution,then cleaned up by PRiME HLB solid-phase extraction cartridge,and samples were separated in PC HILIC column(150 mm×2.0 mm,5μm).The analytes were detected with mass spectrometer in multiple reaction monitoring mode with internal standard.The results showed a good linear in the range of 0.5-50μg/kg for chlorate and perchlorate with the corresponding correlation coefficient 0.9992 and 0.9994.The limit of quantification and detection limit of chlorate in general food were 2.0μg/kg and 0.5μg/kg,respectively,and the limit of quantification and detection limit of perchlorate were 1.0μg/kg and 0.5μg/kg,respectively.The limit of quantification and detection limit of chlorate in packaged drinking water were 0.25μg/kg and 0.50μg/kg,respectively;The limit of quantification and detection limit of perchlorate were 0.25μg/kg and 0.50μg/kg,respectively.The spiked level of 10,20 and 50μg/kg were 80.1%-119.5%,also the mean relative standard deviations was at the range of 2.1%to 9.9%(n=6).This method was suitable for the determination of chlorate and perchlorate in food.