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作 者:冯峰[1] 蒋萍萍[1] 李娜思 周洪斌[3] 储晓刚[1]
机构地区:[1]中国检验检疫科学研究院,食品安全研究所,北京100123 [2]华东理工大学药学院,上海200237 [3]镇江出入境检验检疫局综合技术中心,镇江212008
出 处:《分析化学》2013年第11期1729-1733,共5页Chinese Journal of Analytical Chemistry
基 金:科技部科技支撑计划课题(No.2011BAK10B04);质检总局公益性行业科研专项项目(No.2012104002)资助
摘 要:双氰胺作为乳粉中一种新出现的污染物,对人体特别是婴幼儿的健康有重要影响.本研究建立了快速、准确测定乳粉中双氰胺的超高效液相色谱-电喷雾电离质谱(UPLC-ESI/MS)分析方法.结果表明,采用含2%氨水的乙腈对乳粉样品进行萃取,同时选用UPLC BEH HILIC(150mm×2.1 mm,1.7μm)色谱柱为固定相,以10 mmol/L甲酸铵/甲酸缓冲液(pH 4.0)-乙腈为流动相,梯度洗脱,基质匹配标准曲线定量分析,可以对5~200 μg/L双氰胺样品进行快速准确测定.在ESI正离子模式下,采用选择离子监测方法进行测定时,乳粉中双氰胺的检出限为10 μg/kg.加标浓度在50,100和200 μg/kg样品的回收率分别为83.7%,89.1%和96.7%,相对标准偏差均小于2%.本方法快捷、准确、灵敏度高,可用于乳粉中双氰胺的快速准确测定.Dicyandiamide, as a new contaminant in milk powders, can lead to harmful effects to human health, especially to infants and young children. A rapid and accurate method for the determination of dicyandiamide in milk powders using ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) was established. The milk powders samples were extracted by acetonitrile which contained 2% NH4OH solution ( V/V), the separation was carried out using an UPLC BEH HILIC(150 mm × 2.1 mm, 1.7μm)column, 10 mmol/L ammonium formate/formic acid buffer (pH 4.0) and acetonitrile as the mobile phases, gradient elution. The dicyandiamide was detected by ESI~ under selected ion monitoring mode. The quantified concentration range was 5- 200μg/L using matrix-matched calibration curves. When applying this method to determine real milk powder samples, the detection limits was 10μg/kg. The recoveries were 83.7% , 89.1% and 96.7% respectively when spiked negative samples with 50, 100 and 200 μg/kg dicyandiamide, and the relative standard deviations were less than 2%. This method is rapid, accurate, highly sensitive and suitable for the determination of dicyandiamide in milk powders.
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