鸡蛋中高氯酸盐和氯酸盐残留量的超高效液相色谱-串联质谱测定法

Determination of perchlorate and chlorate in egg by high performance liquid chromatographytandemmass spectrometry

目的建立鸡蛋中高氯酸盐和氯酸盐的超高效液相色谱-串联质谱法。方法用0.1%甲酸水乙腈超声提取,高速离心后,经固相萃取柱净化,过0.22μm滤膜,用Acclaim Trinity P1复合离子交换柱分离,以乙腈-20 mmol/L甲酸铵做流动相,梯度洗脱,采用电喷雾离子源多重反应监测模式测定,同位素内标法定量。结果高氯酸盐在0.1~10.0 g/L内,氯酸盐在1.0~100 g/L内,相关系数均>0.999。高氯酸盐平均回收率范围为94.3%~113.0%,相对标准偏差(RSD)为1.0%~1.7%,检出限为0.1μg/kg,定量限为0.3 g/kg,氯酸盐平均回收率范围为92.8%~102.0%,相对标准偏差(RSD)为0.3%~2.2%,检出限为1.0μg/kg,定量限为3.0 g/kg。结论该方法操作简单、准确、快速、灵敏度高,适用于鸡蛋中高氯酸盐和氯酸盐残留的检测。

Objective To establish a method for the determination of perchlorate and chlorate in egg by high performance liquid chromatography-tandemmass spectrometry.Methods The samples were extracted ultrasonically with 0.1%formic acid water and acetonitrile,purified by solid phase extraction column after high speed centrifugation,filtrated with 0.22μm filter membrane and finally separated with an Acclaim Trinity P1 composite ion exchange column chromatographic column in gradient elution mode with the mobile phase of acetonitrile-20mmol/L ammonium acetate.Electrospray ion source negative ion detection mode(ESI-)and multiple reaction monitoring(MRM)mode were used and the quantifications were based on isotope internal standard method.Results The method had good linearity of perchlorate in the range of 0.1-10.0 g/L and chlorate in the range of 1.0-100 g/L with the correlation coefficients greater than 0.999.The average recovery rates of perchlorate were 94.3%-113.0%with the relative standard deviation(RSD)of 1.0%-1.7%,the detection limit was 0.1μg/kg,and the limit of quantification was 0.3μg/kg.The average recovery rates of chlorate were 92.8%-102.0%with the RSD of 0.3%-2.2%,the detection limit was 1.0μg/kg,and the limit of quantification was 3.0 g/kg.Conclusion The method is simple,accurate,rapid and sensitive,and it is suitable for the determination of perchlorate and chlorate residues in eggs.