摘要
采用超高效液相色谱-串联质谱(UPLC-MS/MS)法测定鱼中孔雀石绿(MG)、隐色孔雀石绿(LMG)、结晶紫(CV)、隐色结晶紫(LCV)残留。样品加入内标,经乙腈涡旋提取、离心、中性氧化铝柱去除脂肪后,氮吹近干,V(乙腈)∶V(5mmol/L醋酸铵)=50∶50的溶液定容,上机测定。MG、CV及其代谢物在4.0μg/L质量浓度范围内有良好的线性关系,MG、LMG、CV的检出限为0.01μg/kg,LCV的检出限为0.06μg/kg。在空白样品中分别添加0.25、2.0μg/kg混合标准溶液和2.0μg/kg内标溶液进行回收率实验,平均回收率在81.4%～97.8%之间,相对标准偏差RSD(n=6)在5.9%～11.2%之间。对109批次实际鱼样进行检测,4种物质均有不同程度的检出。该方法能够灵敏、准确、可靠的测定鱼中MG、LMG、CV、LCV残留,为鱼类水产品养殖、流通及使用环节的市场监管提供参考依据。
Malachite green（MG）, leucomalaehite green（LMG）, crystal violet（CV） and leu- cocrystal violet（LCV） residues in fishes were determinated using ultra-high performance liquid chromatography-mass spectrometry（UPLC-MS/MS）. Samples added with internal standard were firstly extracted and centrifuged in acetonitrile, and then degreased through neutral alumina column, dried in nitrogen, volumed by solution of acetonitrile-5 rnmol/L ammonium acetate （50 ： 50,V/V）. MG, CV and their metabolites have great linearity rela- tionship in the concentration range of 4.0μg/L. The detection limits of MG, LMG and CV are 0. 01 μg/kg, and the LVC is 0. 06 μg/kg. Method recovery is made by addition of 2.0μg/kg internal standard solution and mixed standard solution at concentration levels of 0.25 and 2.0 μg/kg, respectively. The results show that average recoveries are between 81.4% and 97.8%, and relative standard deviations（RSD, n=6） are between 5.9% and 11.2%. These four substances in 109 batches fish samples are detected in different degrees. This method is sensitive and reliable, which can provide reference for market regulators in aquat- ic fish products breeding, using and circulation.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2013年第5期294-299,共6页
Journal of Chinese Mass Spectrometry Society
