论文部分内容阅读
在乳制品的生产过程中,常用季铵盐等消毒剂对生产设备等进行消毒,因此乳制品中存在季铵盐等消毒剂的污染。本文基于QuEChERS净化技术和超高效液相色谱串联质谱(UPLC-MS/MS),建立了一种测定奶粉中5种季铵盐消毒剂残留的新方法。奶粉样品先按比例加水复原成液态乳,然后经乙腈沉淀蛋白,提取液以PSA分散净化后,采用亲水色谱柱(HILIC)分离,在质谱的多反应监测(MRM)模式下测定。结果表明,5种季铵盐在0.2~50μg/L范围内线性关系良好,其相关系数(R)均在大于0.999,奶粉样品的方法检出限(S/N=3)在4.0~14.4μg/kg之间,样品基质的3个添加水平的平均回收率为96.5%~115%,日内精密度(n=6)在3.1%~7.5%之间,日间精密度(n=5)在4.3%~6.7%之间。实际样品检测结果表明奶粉中存在季铵盐消毒剂的残留污染情况。本方法准确灵敏,快速简便,精密度良好,适用于奶粉中以及其他类型乳制品中5种季铵盐消毒剂的分析检检测。
In the production process of dairy products, disinfectants such as quaternary ammonium salts are often used to sterilize production equipment and the like, so that there is contamination of the dairy products with disinfectants such as quaternary ammonium salts. Based on QuEChERS purification technology and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), a new method for the determination of five quaternary ammonium salt disinfectant residues in milk powder was established. The milk powder sample is first replenished into liquid milk proportionally with water, and then the protein is precipitated by acetonitrile. The extract is dispersed and purified by PSA, and then separated by a hydrophilic column (HILIC) and determined by mass spectrometry multiple reaction monitoring (MRM) mode. The results showed that the five quaternary ammonium salts showed a good linearity in the range of 0.2-50 μg / L, the correlation coefficient (R) was above 0.999, and the detection limit (S / N = 3) of milk powder samples was 4.0-14.4 μg / kg, the average recoveries of the three addition levels of the sample matrix were 96.5% -115%, the intra-day precision (n = 6) was between 3.1% and 7.5% 4.3% ~ 6.7% between. The actual sample test results showed residual contamination of quaternary ammonium disinfectant in milk powder. The method is accurate, sensitive, fast and easy, and has good precision. The method is suitable for the analysis and detection of five quaternary ammonium salt disinfectants in milk powder and other types of dairy products.