高效液相色谱-串联质谱法测定肉类中的氯酸盐和高氯酸盐

Determination of Chlorate and Perchlorate Amounts in Meat by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法同时测定肉类中氯酸盐和高氯酸盐的分析方法。样品经乙腈-水(13:7,V:V)提取后离心,上清液经PRiME HLB固相萃取柱净化,Acclaim Trinity P1复合离子交换柱分离,以乙腈及20 mmol/L乙酸铵为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式,内标法定量。结果表明,氯酸盐和高氯酸盐分别在2~200.0 ng/mL、1~100.0 ng/mL范围内呈现良好线性关系,决定系数分别为0.9983和0.9998,方法的定量限分别为2.0、1.0μg/kg。氯酸盐和高氯酸盐分别在三种肉类四个添加水平6.0、20、40、200μg/kg和3.0、10、20、100μg/kg的加标回收率为91.0%~105.7%和94.2%~110.5%,相对标准偏差为1.8%~9.7%和0.7%~9.4%。本方法具有操作简单、灵敏度高、稳定性好等优点,可很好地满足肉中氯酸盐、高氯酸盐的检测。

A method for simultaneous determination of chlorate and perchlorate amounts in meat by high performance liquid chromatography-tandem mass spectrometry was developed.Samples were extracted with acetonitrile/water(13:7,V:V)and centrifuged.The obtained supernatants were purified on a PRiME HLB solid phase extraction column,followed by an Acclaim Trinity P1 ion exchange column with the gradient elution of acetonitrile and 20 mmol/L ammonium acetate as the mobile phase to afford chlorate and perchlorate.MS/MS was performed in ESI+and multiple reaction monitoring mode with an internal standard for quantification.The results showed chlorate and perchlorate had calibration curves with good linearity in the ranges of 2~200.0 ng/mL and 1~100.0 ng/mL respectively,with corresponding correlation coefficients being 0.9983 and 0.9998.The detection limits of the method were 2.0 and 1.0μg/kg,respectively.The recovery rates of chlorate and perchlorate were 91.0%~105.7%and 94.2%~110.5%respectively,at the addition levels of 6.0,20,40,200μg/kg,and 3.0,10,20,100μg/kg.The relative standard deviations for chlorate and perchlorate were 1.8%~9.7%and 0.7%~9.4%respectively.This method would be easy to use and has high detection sensitivity and good stability,and could well meet the requirements of determining chlorate and perchlorate amounts in meat.