鸡蛋中环丙氨嗪及其代谢物三聚氰胺残留检测超高效液相色谱-串联质谱法研究

Determination of Cyromazine and Its Metabolin Melamine Residues in Eggs by UPLC-MS/MS

关键词:  环丙氨嗪  三聚氰胺  鸡蛋  超高效液相色谱－串联质谱法

Key words:  cyromazine  melamine  eggs  UPLC-MS/MS

摘要:

建立了鸡蛋中环丙氨嗪及其代谢物三聚氰胺残留检测的超高效液相色谱－串联质谱（UPLC-MS/MS）方法。液相色谱条件：色谱柱为Waters BEH HILIC柱（50 mm×2.1 mm,1.7 µm）；流动相为乙腈－0.01mol/L乙酸铵溶液，梯度洗脱；柱温30 ℃；流速0.3 mL/min；进样量10 µL。质谱条件为：电喷雾离子源（ESI+），多反应监测（MRM）方式进行采集。结果表明：在2.5~100 μg/L的基质匹配系列混合标准溶液内环丙氨嗪和三聚氰胺的相关系数R2＞0.998；方法检测限为1 μg/L，定量限为2.5 μg/L；从10、50、100 μg/kg三个添加浓度检测结果可以看出，方法的平均回收率为74.6%~91.4%，批内批间RSD值均<15%。

Abstract:

A UPLC-MS/MS method was established for the determination of cyromazine and its metabolin melamine residues in eggs. UPLC condition: the chromatography column is Waters BEH HILIC column of 50 mm×2.1mm,1.7 µm; mobile phase is acetonitrile and 0.01mol/L ammonium acetic; column temperature is 30 ℃; flow rate is 0.3 mL/min；injection volume is 10 µL. Mass spectrometry condition: ESI+ and MRM mode. The calibration curves were good linear between the peak areas and concentrations from 2.5~100 μg/L，the correlation coefficient R2 was higher than 0.998. The detection limit of the method was 1 µg/L, and the limit of quantification was 2.5 µg/L. The average recoveries from spiked samples at the three concentrations of 10, 50, 100 μg/kg ranged from 74.6%~91.4% (n＝5), and intra- and inter-batch variation coefficients were less than 15%.