液质联用法同时测定婴幼儿配方乳粉中氯酸盐和高氯酸盐残留

建立了婴幼儿配方乳粉中氯酸盐和高氯酸盐残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经水超声溶解,乙腈除蛋白。以PC HILIC色谱柱分离,流动相为浓度50 mmol/L的乙酸铵水溶液和乙腈,流速0.25 mL/min。液相色谱-串联质谱仪测定,基质内标法定量。在该优化条件下,氯酸盐和高氯酸定量限分别为20μg/kg和2.0μg/kg,方法回收率为85.1%～94.7%,相对标准偏差(RSD)为2.38%～9.79%。经测定多种市售婴幼儿配方奶粉,表明该方法操作简单、测定结果准确,可用于婴幼儿配方奶粉中氯酸盐和高氯酸盐残留的同时快速测定。

Simultaneous determination of chlorate and perchlorate in infant milk powder by HPLC-MS/MS

A quick confirmative method was developed for determining the residues of chlorate and perchlorate in infant milk powder by HPLC-MS/MS.The sample was ultrasonic extracted with water,Acetonitrile remove protein,N-hexane remove oil.The HPLC separation was carried out on a PC HILIC column,the mobile phase were 50 mmol/L ammonium acetate solution and acetonitrile with isocratic elution,the flow was 0.25 mL/min.Finally the samples were determined by HPLC-MS/MS.Isotope internal matrix-matched calibration was used for the quantification.The limits of quantification(LOQs,S/N=10) of chlorate and perchlorate were 20 μg/kg and 2.0 μg/kg.The overall recoveries varied from 85.1% and 94.7%,and the relative standard deviations(RSD) were 2.38% and 9.79%.The real sample tests showed that the simple and accurate method can be used for determining the residues of chlorate and perchlorate in infant milk powder.