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目的建立乳制品中高氯酸盐的高效液相色谱-串联质谱定量分析检测方法。方法样品采用1%乙酸-乙腈溶液(1∶2,V/V)提取,C18固相萃取柱净化,在IC-Pak~(TM) Anion HR色谱柱(4.6 mm×75 mm,6μm)上,以乙腈-乙酸铵溶液(60∶40,V/V)作为流动相,等度分离。采用液相色谱-质谱联用技术-电喷雾离子源多反应监测模式检测,内标法定量。结果高氯酸盐在0.1~10.0μg/L范围内具有良好的线性关系,牛奶和奶粉的定量限分别为1.0和3.0μg/kg;在三个添加水平下回收率范围在87.6%~122.0%之间,相对标准偏差(RSD)范围为2.0%~10.0%。结论本方法灵敏、准确,适用于乳制品中高氯酸盐的分析测定,具有较好的实际应用价值。
Objective To establish a method for the quantitative analysis of perchlorate in dairy products by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 1% acetic acid-acetonitrile (1: 2, V / V) and purified on a C18 solid-phase extraction column. On an IC- Pak ™ Anion HR column (4.6 mm × 75 mm, 6 μm) With acetonitrile-ammonium acetate solution (60:40, V / V) as the mobile phase, the same separation. Using liquid chromatography - mass spectrometry technology - electrospray ionization multiple reaction monitoring mode detection, internal standard method. Results Perchlorate had a good linearity in the range of 0.1 ~ 10.0 μg / L with the limits of quantitation of 1.0 and 3.0 μg / kg for milk and milk powder, respectively. The recoveries ranged from 87.6% to 122.0% The relative standard deviation (RSD) ranged from 2.0% to 10.0%. Conclusion The method is sensitive and accurate and suitable for the determination of perchlorate in dairy products, which has a good practical value.