中国广州分析测试中心广东省分析测试技术公共实验室
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黄芳, 马叶芬, 吴惠勤, 等. 液相色谱-串联质谱法快速测定奶粉中的双氰胺[J]. 分析测试学报, 2013,32(3):271-274.
Determination of Dicyandiamide in Infant Milk Powder by LC-MS/MS[J]. 2013,32(3):271-274.
建立了奶粉中双氰胺的高效液相色谱-串联质谱快速测定方法。实验优化了前处理条件、液相色谱条件和质谱参数。样品经水提取,乙腈分次沉淀蛋白后,采用亲水高效液相色谱柱分离,流动相为乙腈(含0.2%甲酸)-0.1%甲酸(含10 mmol/L甲酸铵)(体积比95∶5),流速0.3 mL/min。采用正离子模式的电喷雾质谱检测,多反应(MRM)选择离子监测,检测离子对为m/z 85→68和m/z 85→43,检测周期为5 min。结果显示,双氰胺在0.2~100 μg/L范围内线性良好,相关系数为0.999 8。双氰胺的检出限为0.1 μg/L,方法的定量下限为5 μg/kg。低、中、高3个加标水平下的平均回收率为79%~83%,相对标准偏差为2.7%~6.5%。方法简便快速、准确可靠,已用于奶粉中双氰胺的检测。
A method was developed for the determination of dicyandiamide in infant milk powder by high-performance liquid chromatography-mass spectrometry(LC-MS/MS).The conditions of extraction and parameters of LC-MS were optimized.The sample was extracted with water,precipitated with acetonitrile,then separated on a Thermo syncronis column using mixture of acetonitrile(containing 0.2% formic acid)-0.1% formic acid(containing 10 mmol/L ammonium formate)(95∶5) as mobile phase at a flow rate of 0.3 mL/min.The detection of dicyandiamide was performed by positive-ion electrospray ionization mass spectrometry(ESI-MS) utilizing multiple reaction monitoring of two parent-daughter ion pairs:m/z 85/68 and 85/43.A good linear relationship was obtained in the range of 0.2-100 μg/L,with a correlation coefficient of 0.999 8.The spiked recoveries at different spiked levels were in the range of 79%-83%.The detection limit of dicyandiamide was 0.1 μg/L,and the quantitatiion limit of method was 5 μg/kg.The results indicated that the method was rapid,selective,sensitive and stable enough to examine dicyandiamide in infant milk powder.
双氰胺液相色谱-串联质谱奶粉
dicyandiamideliquid chromatography-mass spectrometry(LC-MS/MS)infant milk powder
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