QuEChERS-超高效液相色谱-串联质谱法测定水果中高氯酸盐

Determination of perchlorate in fruit by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  高氯酸盐  超高效液相色谱-串联质谱  水果  QuEChERS

英文关键词:perchlorate  ultra performance liquid chromatography-tandem mass spectrometry  fruit  QuEChERS

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定水果中高氯酸盐的分析方法。方法 水果样品经乙腈-水(1:1, V:V)提取, C18和石墨化炭黑(graphitized carbon black, GCB)净化后, Waters Torus DEA色谱柱 (100 mm×2.1 mm, 1.7 μm)分离, 用0.9%(V:V)甲酸乙腈-50 mmol/L甲酸铵(pH=2.9)溶液进行梯度洗脱, 电喷雾负离子模式下, 多反应监测(multiple reaction monitoring, MRM)模式进行测定, 内标法定量。结果 高氯酸盐在0.5~20 μg/L浓度范围内呈良好的线性关系, 相关系数r=0.9987, 方法检出限为0.8 μg/kg, 定量限为 2.5 μg/kg。在浓度分别为10、20、100 μg/kg加标水平下, 高氯酸盐的回收率为87.7%~102%, 相对标准偏差小于6.1%。结论 该方法简单快捷、准确可靠, 适用于水果中高氯酸盐的测定。

英文摘要:

      Objective To establish a method for the determination of perchlorate in fruit by QuEChERS- ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile-water(1:1, V:V), cleaned up with C18 powder and graphitized carbon black powder, separated on a Waters Torus DEA column (100 mm×2.1 mm, 1.7 μm)with gradient elution using acetonitrile containing 0.9% formic acid and 50 mmol/L ammonium acetate(pH=2.9), and detected by negative ion electrospray ionization mass spectrometry under multiple reaction monitoring(MRM) mode, and then quantitatively detected with internal standard method. Results The calibration curve showed a good linear in the range of 0.5?20 μg/L, and the correlation coefficient was 0.9987. The limit of detectionwas 0.8 μg/kg and the limit of quantification was 2.5 μg/kg. At spiked levels of 10, 20, 100 μg/kg (n=6), the recoveries of perchlorate were 87.7%?102%. The relative standard deviations were less than 6.1%. Conclusion This method is simple and sensitive, which can be used for the analysis of perchlorate in fruit.