UPLC-MS/MS法测定新疆冷水鱼中孔雀石绿与隐色孔雀石绿  

Determination of Malachite Green and Leuco Malachite Green in Cold Water Fish in Xinjiang by UPLC-MS/MS MethodUPLC-MS/MS

作　　者：李晓岩[1] 武运[2] 王犁烨 苏敏[1] 沈慧慧[1] 巴哈提古丽·马那提拜[1] LI Xiao-yan;WU Yun;WANG Li-ye;SU Min;SHEN Hui-hui;Bakhetgul Manatbay(Inspection and Quarantine Technology Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau,Urumqi 830063,China;College of Animal Sciences,Xinjiang Agricultural University,Urumqi 830052,China)

机构地区：[1]新疆出入境检验检疫局技术中心,乌鲁木齐830063 [2]新疆农业大学,乌鲁木齐830052

出　　处：《新疆农业科学》2019年第7期1328-1334,共7页Xinjiang Agricultural Sciences

基　　金：国家质量监督检验检疫总局科研项目(2007IK174)~~

摘　　要：【目的】建立新疆冷水鱼中孔雀石绿(MG)和隐色孔雀石绿(LMG)残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)更为简便、高效的检测方法。【方法】样品经1%冰乙酸-乙腈溶液提取,氨基及SCX(强阳离子交换)固相小柱净化,C18色谱柱分离,电喷雾串联四极杆质谱的多反应监测扫描模式(MRM)进行检测,并采用内标法定量。【结果】MG和LMG在5.0~100.0μg/L线性范围内具有良好的线性关系,相关系数分别为:0.999 7(MG)和0.999 2(LMG)。测定低限(LOQ)为2.0μg/kg。以空白样品为基体做加标回收,测得MG的回收率在88%~105%,LMG的回收率在85%~110%,相对标准偏差(n=6)均为2.2%~15.3%。【结论】该方法样品前处理简便,回收率高,稳定性好。适用于新疆冷水鱼中MG和LMG残留量的日常检测。【Objective】This project aims to establish a more convenient ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of malachite green(MG)and leuco malachite green(LMG)residues in cold water fish in Xinjiang.【Method】The sample was extracted with 1%glacial acetic acid-acetonitrile solution,purified by amino and SCX(strong cation exchange)solid phase cartridges,separated by C18 column,and multi-reaction monitoring scanning mode(MRM)of electrospray ionization tandem mass spectrometry,detected and quantified by internal standard method.【Result】MG and LMG had a good linear relationship in the linear range of 5.0-100.0μg/L,and the correlation coefficients were 0.999,7(MG)and 0.999,2(LMG),respectively.The lower limit of determination(LOQ)was 2.0μg/kg.The test was carried out by adding blank sample as the matrix.The recovery rate of MG was 88%-105%,the recovery rate of LMG was 85%-110%,and the relative standard deviation(n=6)was 2.2%-15.3%.【Conclusion】The method has the advantages of simple pretreatment,high recovery rate and good stability,whcih is suitable for routine testing of mg and lmg residues in cold water fish in Xinjiang.

关 键 词：超高效液相色谱-串联质谱 新疆冷水鱼 孔雀石绿 隐色孔雀石绿 

分 类 号：S911[农业科学—水产科学]