超高效液相色谱-串联质谱法检测芹菜和土壤中灭蝇胺及其代谢物三聚氰胺残留

Determination of cyromazine and its metabolite melamine residues in celery and its soil by ultra performance liquid chromatography tandem mass spectrometry

目的建立超高效液相色谱-串联质谱测定芹菜和土壤中灭蝇胺及其代谢物三聚氰胺残留的分析方法。方法样品以甲醇:水=4:1(V:V)混合溶液提取,经混合阳离子固相萃取柱净化,亲水作用色谱柱分离,以10mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱,通过电喷雾离子源正离子检测模式和多重反应监测模式测定,同位素内标法定量。结果灭蝇胺和三聚氰胺在0.01~1.0 mg/L范围内线性关系均较好,检出限为8.16×10–6~6.91×10–5 mg/kg,在0.01、0.1和1.0 mg/kg 3个添加水平下,方法回收率在81.96%~108.81%,相对标准偏差为2.83%~6.19%(n=5)。结论该方法简单、快速、准确,适合用于芹菜和土壤中灭蝇胺及其代谢物三聚氰胺的定性和定量检测。

Objective To establish a method for the determination of cyromazine and melamine residues in celery and its soil by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods The sample was extracted with methanol: water =4:1(V:V) mixed solution, purified with mixed cationic solid phase extraction column, separated with hydrophilic chromatography column by gradient elution using 10 mmol/L ammonium acetate solution and acetonitrile as mobile phases, detected by electrospray ion source positive ion detection mode and multiple reaction monitoring mode, and quantified by isotope internal standard method. Results Cyromazine and melamine had a good linear relationship in the concentration range of 0.01–1.0 mg/L. The limits of detection were 8.16×10–6–6.91×10–5 mg/kg. The average recoveries were ranged from 81.96% to 108.81% for cyromazine and melamine at 3 spiked levels of 0.01, 0.1 and 1.0 mg/kg. The relative standard deviations were less than 6.19%(n=5). Conclusion This method is simple, rapid and accurate, and is suitable for the qualitative and quantitative determination of cyromazine and its metabolite melamine in celery and soil.