摘要
建立了冰鲜三文鱼中孔雀石绿及其代谢物残留量的高效液相色谱-串联质谱分析方(HPLCMS/MS)。样品在抗坏血酸的保护下,采用乙睛-乙酸鞍溶液超声提取,氯化钠盐析、C18填料除脂,中性氧化铝填料分散固相萃取吸附极性干扰物。孔雀石绿及其代谢物在乙睛-0.1%甲酸组成梯度洗脱流动相中采用C18色谱柱分离,在电喷雾正电离多反应模式下监测,内标法定量。结果表明样品中孔雀石绿及其代谢物残留在0.5μg/kg?20 μg/kg之间时,线性相关系数大于0.998,方法检出限(LOD,S/NM3)为0.1 μg/kg,定量限(LOQ,S/NM10)为0.5μg/kg,3个不同添加水平时回收率为87.6%~105.7%,相对标准偏差(RSD)在3.3%~7.5%之间。经测定实际样品,证明该方法简便、快速、准确,可以满足冰鲜三文鱼中孔雀石绿及其代谢物分析要求。
An analytical method was developed for determination of malachite and its metabolites residues in chilled salmon by high performance liquid chromatography tandem mass spectrometry.The samples were extracted with acetonitrile and ammonium acetate solutions.Under the condition of NaCl salting out,C18 was used for removing fat.Neutral alumina dispersive solid phase extraction dispersion solid phase extraction(DSPE)was introduced to cleanup procedures.The separation was performed on a C18 column under a gradient elution using acetonitrile and 0.1%formic acid.The analytes were detected in the positive multi-reaction monitoring(MRM)mode.The quantification was carried out on internal standards.In the concentration ranges of 0.5μg/kg-20μg/kg,the correlation coefficients for malachite green and its metabolite were not less than 0.998.The limit of detection(LOD,SZZVM3)was 0.1μg/kg and the limits of quantification(LOQ,S//VM10)was 5μg/kg.The recoveries of malachite green and its metabolite spiked at different levels ranged from 87.6%to 105.7%with the relative standard deviations within the range of 3.3%-7.5%.The results analyzed by various real samples showed that the method was simple,rapid,accurate and suitable for the determination of malachite green and its metabolites residue in salmon.
作者
祝伟霞
孙转莲
张丹
冯景菲
杨娜
Zhu Weixia;Sun Zhuanlian;Zhang Dan;Feng Jingfei;Yang Na(Zhengzhou Customs Technology Center,Zhengzhou 450003)
出处
《河南水产》
2019年第5期20-23,共4页
HENAN FISHERIES
基金
海关总署科研项目基于氨基酸功能因子指纹同位素技术研究进口三文鱼的溯源鉴定(2019HK102)
河南省科技攻关项目(172102310558).
关键词
液相色谱-串联质谱
分散固相萃取
孔雀石绿及其代谢物
冰鲜三文鱼
liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
dispersion solid phase extraction(DSPE)
malachite green and its metabolites
chilled salmon
