高效液相色谱-串联质谱法测定大米中高氯酸盐含量

Determination of perchlorate in rice by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  电喷雾离子源  大米  高氯酸盐

英文关键词:high performance liquid chromatography-tandem mass spectrometry  electrospray ionization  rice  perchlorate

中文摘要:

      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0.3 mL/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4.0 μg/kg, 定量限为10.0 μg/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。

英文摘要:

      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.