反相超高效液相色谱-串联质谱法测定大米中氯酸盐和高氯酸盐

Determination of chlorate and perchlorate in rice by reversed-phase ultra performance liquid chromatography-tandem mass spectrometry

目的建立反相超高效液相 -串联质谱 (high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定大米中氯酸盐和高氯酸盐的方法。方法大米样品采用水和甲醇提取,经固相萃取(solid-phase extraction, SPE)净化,在电喷雾离子源负离子多反应监测(multiple reaction monitoring, MRM)模式下进行测定,内标法定量。结果 氯酸盐和高氯酸盐在 1.00~200 ng/m L 范围内线性关系良好(r>0.9955), 方法检出限为 4.0~6.0 μg/kg。添加水平分别为 12.5、25、50 μg/kg 时,加标回收率为 82.7%~99.5%, 相对标准偏差为 1.01%~7.90%。结论 该方法简便、灵敏度高,适用于大米中氯酸盐和高氯酸盐的检测。

Objective To establish a method for the determination of chlorate and perchlorate in rice by reversed-phase ultra performance liquid chromatography-tandem mass spectrometry. Methods The rice samples were extracted with water and methanol, and purified by solid-phase extraction(SPE). The samples were determined by multiple reaction monitoring(MRM) mode under electrospray ionization and quantified by internal standard method. Results The linear relationship between chlorate and perchlorate in the range of 1.00-200 ng/mL was good(r>0.9955), and the detection limit of the method was 4.0-6.0 μg/kg. When the addition levels were 12.5, 25, 50 μg/kg, the recoveries were 82.7%-99.5%, and the relative standard deviations were 1.01%-7.90%. Conclusion The method is simple, sensitive, which is suitable for the detection of chlorate and perchlorate in rice.