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1、超高效液相色谱法快速测定水产品中孔雀石绿、结晶紫的含量刘少彬*,胡浩光,谢翠美,莫炯怀(东莞市海洋与渔业环境监测站,东莞523079)摘要:目的建立超高效液相色谱(ultraperformanceliquidchromatography,UPLC)测定水产品中孔雀石绿、结晶紫的含量。方法样品经加酸性氧化铝净化、乙腈旋涡振荡、硼氢化钾还原,超声提取,提取液真空浓缩近干后用乙腈溶解残渣。残渣液过串联酸性氧化铝AL-A柱和丙磺酸PRS柱,净化过程中在移除AL-A柱后,用3mL水淋洗PRS柱,最后用乙酸铵和乙
2、腈(1:1,V:V)洗脱,过滤供UPLC测定。结果孔雀石绿和结晶紫在0.5~500μg/L浓度范围内呈现良好的线性关系。GB/T20361-2006经改进后,回收率和重复性均满足国标方法的要求。结论该方法简便、准确、高效,适用于水产品中孔雀石绿和结晶紫残留量的快速检测。关键词:超高效液相色谱法;孔雀石绿;结晶紫;水产品Rapiddeterminationofmalachitegreenandcrystalvioletinaquaticproductsbyultraperformanceliquidch
3、romatographyLIUShao-Bin*,HUHao-Guang,XIECui-Mei,MOJiong-Huai(DongguanMarineandFisheryEnvironmentMonitoringStation,Dongguan523079,China)ABSTRACT:ObjectiveToestablishamethodfordeterminationofmalachitegreenandcrystalvioletinaquaticproductbyultraperformance
4、liquidchromatography(UPLC).MethodsSampleswerecleanedwithacidicalumina,vortexoscillatedwithacetonitrile,processedwithpotassiumborohydridereductionandultrasonicextraction.Theextractwasvacuumconcentrateduntilneardryandtheresiduewasdissolvedwithacetonitrile
5、.TheresidueliquidpassedseriesAL-AandPRScolumnsforpurificationprocess,3mLwaterwasusedtoleachPRScolumnaftertheremovalofAL-A,andfinallyammoniumacetateandacetonitrile(1:1,V:V)wereusedforelution.andthenthefiltratewasdeterminedbyUPLC.ResultsMalachitegreenandc
6、rystalviolethadgoodlinearrelationshipsintherangeof0.5~500μg/L.AftertheimprovementofGB/T20361-2006,therecoveryandrepeatabilityofthemethodcouldmeettherequirementsofthenationalstandardmethod.ConclusionTheestablishedmethodissimple,accurateandefficient,which
7、issuitableforrapiddetectionofmalachitegreenandcrystalvioletresiduesinaquaticproduct.KEYWORDS:ultraperformanceliquidchromatography;malachitegreen;crystalviolet;aquaticproducts1引言孔雀石绿(malachitegreen,MG)属于三苯甲烷类染料,自20世纪30年代早期,孔雀石绿就在养殖场作为常用抗感染药物使用[1]。结晶紫(cry
8、stalviolet,CV)又称六甲基紫,是一种带有金属光泽的深绿色固体,易溶于水,具有杀菌作用,其结构性质与孔雀石绿相似[2,3]。鱼接触了孔雀石绿和结晶紫水溶液后,会被鱼体吸收并分布到不同的组织,并代谢成简单的隐色化合物-隐色孔雀石绿(leucomalachitegreen,LMG)和隐色结晶紫(leucocrystalviolet,LCV),隐色孔雀石绿和隐色结晶紫残留十分稳定,在鱼体内和环境中残留时间长[4-9]。而水产品味道鲜美,营养丰富,随着
