摘要
目的建立高效液相色谱-串联质谱法测定大米中高氯酸盐的含量。方法样品提取液经过固相萃取柱快速净化处理后去除基质干扰物,采用Thermo Acclaim TRINITY P1色谱柱分离,以乙腈-20 mmol/L甲酸铵为流动相进行梯度洗脱,流速为0.3mL/min,柱温30℃,外标法定量检测。结果在高氯酸盐浓度为1.0～100.0 ng/mL的范围内的线性相关系数较好(r=0.999),检出限为4.0μg/kg,定量限为10.0μg/kg,高、中、低3个浓度水平的加标回收率在82.3%～93.2%之间,测定值的相对标准偏差小于5%(n=6)。结论该方法简便快捷、灵敏可靠,适用于大米中高氯酸盐的快速检测。
Objective To establish a method for determination of perchlorate in rice by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The sample extract was quickly purified by a solid phase extraction column to remove matrix interferences. The samples were separated with a Thermo Acclaim TRINITY P1 column at the flow rate of 0.3 mL/min by gradient elute using acetonitrile and 20 mmol/L ammonium formate as mobile phase. The flow rate was 0.3 mL/min, and the column temperature was 30 ℃. The external standard method was used for quantitative determination. Results The linear correlation coefficient was good in the range of perchlorate concentration of 1.0 to 100.0 ng/mL(r=0.999). The limit of detection of method was 4.0 μg/kg,and the limit of quantification of method was 10.0 μg/kg. When the recoveries at 3 levels ranged from 82.3% to 93.2%, the values of the relation standard deviation were less than 5%(n=6). Conclusion This method is simple,rapid, sensitive and reliable, and is suitable for the rapid detection of perchlorate in rice.
引文
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