超高效液相色谱-串联质谱法检测鱼中孔雀石绿、结晶紫及其代谢物  

Determination of Malachite Green, Crystal Violet and Their Metabolites in Fishes by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张艺蓓[1] 岳田利[1] 乔海鸥[2] 贾如[1] 蒋旭鹏[1] 李璐[1] 

机构地区：[1]西北农林科技大学食品科学与工程学院,陕西杨凌712100 [2]陕西省疾病预防控制中心,陕西西安710054

出　　处：《食品科学》2014年第10期179-184,共6页Food Science

基　　金：2013年度西北农林科技大学"大学生创新创业训练计划"校级重点项目(1201310712174)

摘　　要：采用超高效液相色谱-串联质谱法同时测定鱼中孔雀石绿（malachite green,MG）、隐性孔雀石绿（leuco malachite green,LMG）、结晶紫（crystal violet,CV）、隐性结晶紫（leuco crystal violet,LCV）4种物质残留。样品加入内标物D5-MG、D6-LMG、D5-CV、D6-LCV,经乙腈提取、离心、过中性氧化铝柱,氮气吹至近干,50%乙腈溶液定容,上机测定。MG和LMG线性范围为1-50ng/mL,CV和LCV线性范围为1-100ng/mL。4种物质的检出限均为0.05μg/kg,定量限均为0.15μg/kg。在50、100、200 ng/mL 3个添加水平下,回收率在87.80%-110.82%之间,相对标准偏差均小于等于4.32%（n=6）。该方法灵敏、准确、可靠,可以同时测定鱼中MG、LMG、CV、LCV残留。Purpose： Malachite green （MG）, leuco malachite green （LMG）, crystal violet （CV） and leuco crystal violet （LCV） residues in fish were determined simultaneously using ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS-MS）. Methods： Fish samples after addition of internal standards D5-MG, D6-LMG, D5-CV, and D6-LCV were extracted with acetonitrile and centrifuged, and then the supernatants were applied on a neutral alumina column, blown almost dry under a stream of nitrogen and re-dissolved in 50% aqueous acetonitrile （by volume） before being subjected to UPLC-MS-MS analysis. Results： A linear relationship was observed over a concentration range of 1-50 ng/mL for MG and LMG, and over a concentration range of 1-100 ng/mL for CV and LCV. The limits of detection （LOD） for MG, LMG, CV and LCV were 0.05 μg/kg and the limits of quantification （LOQ） for all of them were 0.15 μg/kg. Average recoveries from blank samples spiked at levels of 50, 100 and 200 ng/mL ranged from 87.80% to 110.82%, with relative standard deviation smaller than or equal to 4.32% （n = 6）. Conclusions： This method proved sensitive, accurate and reliable.

关 键 词：超高效液相色谱-串联质谱 鱼 孔雀石绿 结晶紫 残留 

分 类 号：TS207.3[轻工技术与工程—食品科学]