婴配乳粉基氯酸盐和高氯酸盐标准样品的研制与评估

Preparation and Evaluation of Chlorate and Perchlorate Reference Material in Infant Formula Milk Powder

婴幼儿配方乳粉中氯酸盐、高氯酸盐污染会影响婴幼儿的正常生长和发育,氯酸盐和高氯酸盐的检测已有相关标准,但我国尚缺乏婴幼儿配方乳粉氯酸盐和高氯酸盐检测的乳粉基标准样品。通过乳粉基质中氯酸盐和高氯酸盐的精确添加,以低进风温度喷雾干燥和真空干燥复合干燥技术制备标准样品;选用乙腈沉淀蛋白-高效液相色谱-串联质谱高精度检测方法对标准样品进行均匀性检验和稳定性监测。采用单因素方差分析对均匀性检验结果进行评估,采用t-检验法,对-25, 0, 20和40℃梯度温度为期1周的稳定性监测以及0, 0.5, 1, 3, 6和12个月室温的长期稳定性监测结果进行评估。结果证明,标准品的均匀性、稳定性良好,氯酸盐和高氯酸盐目标制备值与测得值吻合。

Chlorate and perchlorate in infant formula milk powder will affect the normal growth and development of infants and young children. There were already standards for the detection method of chlorate and perchlorate, but there was no chlorate and perchlorate reference material for testing. The reference materials were prepared by the matrix addition-low inlet air temperature spray drying and vacuum drying composite drying technology. The method of acetonitrile-precipitated protein-high performance liquid chromatography-tandem mass spectrometry was used to perform uniformity test and stability monitoring on reference material. The single factor analysis of variance was used to evaluate the homogeneity test results, and the homogeneity of reference material was good. Four gradient temperatures of-25, 0, 20 and 40 ℃ were used to monitor the stability of the reference material for one week and long-term stability monitoring for 0, 0.5, 1, 3, 6 and 12 months. The t-test was used to evaluate the stability of reference material. The stability of reference material was good. The research showed that the target preparation value of chlorate and perchlorate in the sample was consistent with the measured value.