摘要
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.
作者
代艳娜
刘青海
蒲继锋
央珍
潘虎
张一帆
DAI Yan-Na;LIU Qing-Hai;PU Ji-Feng;YANG Zhen;PAN Hu;ZHANG Yi-Fan(Institute of Agricultural Product Quality Standard and Testing Research,Tibet Academy of Agricultural and Animal Husbandry Sciences,Lhasa 850032,China)
出处
《食品安全质量检测学报》
CAS
2020年第15期5020-5026,共7页
Journal of Food Safety and Quality
基金
西藏自治区自然科学基金项目(XZ2019ZRG-91)
西藏自治区科技厅重点研发与转化项目(XZ201801NB07)
国家农产品质量安全风险评估专项(GJFP2019007)
西藏自治区财政专项(XZNKYZBS-2020-C-029)。
关键词
同位素内标
超高效液相色谱-串联质谱法
灭蝇胺
三聚氰胺
芹菜
土壤
isotope-labeled internal standard
high performance liquid chromatography-tandem mass spectrometry
cyromazine
melamine
celery
soil