PRiME HLB固相萃取-超高效液相色谱-串联质谱法测定水产品中的孔雀石绿含量
Determination of Malachite Green in Aquatic Products by Ultra-high Performance Liquid Chromatography Mass Spectrometry Coupled with PRiME HLB Solid Phase Extraction
欧柏尧 1宋海霞 1梁莹 1赵天珍1
作者信息
- 1. 中山市农产品质量安全检验所,广东中山 528400
- 折叠
摘要
目的:建立了水产品中显色孔雀石绿(MG)及隐色孔雀石绿(LMG)残留量的超高效液相色谱-串联质谱测定方法.方法:样品用1.5％甲酸乙腈提取,离心,提取液经过PRiME HLB通过式固相萃取柱净化,氮吹后复溶,UPLC-MS/MS测定,同位素内标法定量.结果:在浓度为0.5～10.0μg/L范围内线性关系均良好,相关系数均大于0.995,检测限为0.008～0.01μg/kg,定量限为0.02～0.04μg/kg,加标回收率为86.8％～110.5％,相对标准偏差为1.6％～5.8％.结论:该方法高效快捷、准确可靠,能够满足大批量水产品中孔雀石绿及隐色孔雀石绿的检测.
Abstract
Objective:The method for determinatiom Malachite Green(MG) and Leumalachite Green(LMG) in aquatic products by using Ultra-high Performance Liquid Chromatography Mass Spectrometry(UPLC-MS/MS)in combination with pass-through column was established.Method:The drugs in the sample were extracted with 1.5％ formic acid acetonitrile,centrifuged,and the extractionwas purified through a PRiME HLB solid-phase extraction column. After nitrogen blowing,it was redissolved and determined by UPLC-MS/MS,followed by quantitative analysis using isotope internal standard method. Results:The linear relationships of the drugs were good within the concentration range of 0.5～10 μg/L,with corre-lation coefficients greater than 0.995. The detection limit is 0.008～0.01 μg/kg,with a quantification limit of 0.02～0.04 μg/kg.The recovery rate for spiking is 86.8％～110.5％,with a relative standard deviation of 1.6％～5.8％. Conclusion:This method is simple,efficient,with good precision and accuracy,and can meet the requirements for the detection of Mala-chite Green and Leumalachite Green in large quantities of samples aquatic products.
关键词
孔雀石绿/水产品/PRiME/HLB/超高效液相色谱-串联质谱Key words
Malachite Green/aquatic products/PRiME HLB/ultra-high perfoemance liquid chromatography mass spectrometry引用本文复制引用
出版年
2024
NETL
NSTL
万方数据