摘要
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。
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.
作者
王浩
贾婧怡
张杉
张旭
陈江龙
赵丽
WANG Hao;JIAJingyi;ZHANG Shan;ZHANG Xu;CHENG Jianglong;ZHAO Li(China National Food & Safety Supervision and Inspection Center,Beijing 100094,China)
出处
《中国乳品工业》
CAS
北大核心
2019年第2期48-50,64,共4页
China Dairy Industry
基金
北京市科研专项资助项目(Z171100004417026)
