【摘要】 建立了同时测定奶粉中双氰胺与三聚氰胺含量的高效液相色谱-串联质谱法。采用CAPCELL PAK CR 1:4色谱柱(2.0 mm i.d×150 mm,5μm),V(乙腈):V(CH3COONH4溶液,2 mmol/L,用乙酸调pH=4)=95:5为流动相,流速0.3 mL/min,柱温35℃,质谱检测器进行检测,外标法定量。在上述条件下,两种目标化合物在10~500 ng/mL范围内,质量浓度与定量离子峰面积呈良好的线性关系。对奶粉样品进行添加回收,双氰胺与三聚氰胺的平均回收率分别为93.4%~97.0%,92.7%~98.1%,相对标准偏差(RSD)分别为3.7%~5.8%,3.4%~5.7%。该方法可用于奶粉样品中双氰胺与三聚氰胺含量的分析。更多还原

【Abstract】 A method for the determination of dicyandiamide and melamine in powder milk by high performance liquid chromatography-tandem mass spectrometry was developed.The samples were separated on a CAPCELL PAK CR 1∶ 4 column(2.0 mm i.d × 150 mm,5 μm) with 95% acetonitrile + 5% 2 mmol ammonium acetate(pH = 4) as THE mobile phase at a flow rate of 0.3 mL / min,and detected by mass spectrometry.The target compounds were successfully separated from relevant impurities under the conditions mentioned above.The calibration curve was linear in the range of 10 ~ 500 ng / mL.The average recoveries of dicyandiamide and melamine were 93.4% ~ 97.0% and 92.7% ~ 98.1%,and the relative standard deviations(RSD) were 3.7% ~ 5.8% and 3.4% ~ 5.7%,respectively.The method is simple,rapid and suitable for the determination of dicyandiamide and melamine in powder milk.更多还原