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

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。

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

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 1.0 μg/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, 200 μg/kg, and 3.0, 10, 20, 100 μg/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.