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 Chro⁃matography Mass Spectrometry Coupled with PRiME HLB Solid Phase Extraction

作　　者：欧柏尧 宋海霞 梁莹 赵天珍 OU Bai-yao;SONG Hai-xia;LIANG Ying;ZHAO Tian-zhen(Zhongshan Quality Safety&Inspection Institute of Agricultural Products,Zhongshan 528400,China)

机构地区：[1]中山市农产品质量安全检验所,广东中山528400

出　　处：《安徽化工》2024年第4期146-149,共4页Anhui Chemical Industry

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。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 0.5~10μg/L,with corre‐lation coefficients greater than 0.995.The detection limit is 0.008~0.01μg/kg,with a quantification limit of 0.02~0.04μg/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 

分 类 号：O657[理学—分析化学]