高效液相色谱-串联质谱法测定再制干酪中的三聚氰胺

Determination of melamine in processed cheese by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  再制干酪  三聚氰胺

英文关键词:high performance liquid chromatography-tandem mass spectrometry  processed cheese  melamine

中文摘要:

      目的 建立高效液相色谱-串联质谱法准确、快速检测再制干酪中三聚氰胺的方法。方法 样品中的三聚氰胺经2%的三氯乙酸溶液提取, 乙酸铅沉淀蛋白、正己烷脱脂后, 经CX固相萃取柱净化, 通过高效液相色谱串联三重四极杆质谱联用仪进行测定, 外标法定量。结果 三聚氰胺含量在50~300 ng/mL的范围内与峰面积有良好的线性关系, 相关系数为0.9999, 方法定量限为10 μg/kg。添加水平为10、50、100、200 μg/kg的奶酪样品加标回收率为81.4%~103.2%, 测定结果的相对标准偏差均小于7%(n=6)。结论 该方法操作简便、定量准确、经济, 适用于儿童奶酪等多种再制干酪产品中三聚氰胺测定。

英文摘要:

      Objective To establish a method for the accurate and rapid determination of melamine in processed cheese by high performance liquid chromatography-tandem mass spectrometry. Methods The melamine in the sample was extracted with 2% trichloroacetic acid solution, protein was precipitated by lead acetate, and the n-hexane was used for degreasing, then purified by CX solid phase extraction column. The samples were determined by high performance liquid chromatography tandem triple quadrupole mass spectrometer and quantified by external standard method. Results Melamine had good relationship with peak area in the range of 50–300 ng/mL, with the correlation coefficient of 0.9999. The limit of quantification for melamine was 10 μg/kg. The average recoveries ranged from 81.4%–103.2% at the spiked levels of 10, 50, 100 and 200 μg/kg with the relative standard deviation of determination results less than 7% (n=6). Conclusion This method is simple, quantitatively accurate and economical, and is suitable for melamine determination in a variety of processed cheese products, such as children's cheese.