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

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,1.7μm)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0.5~20μg/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0.8μg/kg,定量限为2.5μg/kg。在浓度分别为10、20、100μg/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。

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,1.7μm)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 0.5-20μg/L,and the correlation coefficient was 0.9987.The limit of detectionwas 0.8μg/kg and the limit of quantification was 2.5μg/kg.At spiked levels of 10,20,100μg/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.