液相色谱-串联质谱法同时测定水产品中孔雀石绿、结晶紫以及它们的隐色代谢物残留  

Simultaneous Determination of Residues of Malachite Green,Crystal Violet and Their Leuco Metabolites in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：朱宽正[1] 王鹏[1] 林雁飞 萧松建[1] 梅素容[1] 

机构地区：[1]华中科技大学同济医学院公共卫生学院环境医学研究所教育部环境与健康重点实验室 [2]湖北出入境检验检疫局,湖北武汉430022

出　　处：《色谱》2007年第1期66-69,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金(No.20407009);湖北省自然科学基金(No.2003ABA060)资助项目

摘　　要：采用液相色谱-串联质谱法（LC—MS／MS）同时测定水产品中的孔雀石绿、结晶紫以及它们的隐色代谢物残留。匀质后的水产品样品用乙腈和乙酸铵缓冲液提取。合并提取液，用二氯甲烷反提取，经中性氧化铝柱和PRS柱固相萃取净化。采用ZORBAX SB—C18色谱柱，并以0．5mmol／L乙酸铵-乙腈（体积比为10：90）混合溶液为流动相，无需使用氧化铅柱在线氧化，色谱分离后直接进入串联质谱检测器检测。采用电喷雾离子源，正离子多反应监测（MRM）模式检测。方法的检测限（S／N=3）可达0．5ng／g，平均加标回收率为77．6％～98．1％，相对标准偏差均小于8．2％。大量实际水产品样品的检测结果表明，此方法适合于对水产品中孔雀石绿、结晶紫以及它们的隐色代谢物的残留检测。A liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was developed for the simultaneous determination of the residues of malachite green （ MG）, eucomalachite green （LMG）, crystal violet （CV） and leucocrystal violet （LCV） in aquatic products. The target analytes were extracted from homogenized samples with a mixture of acetonitrile and ammonium acetate buffer, partitioned against methylene chloride, and purified on tandem neutral alumina and PRS solid-phase extraction （SPE） cartridges. Chromatographic separation was achieved by using a ZORBAX SB-C18 column with an isocratic mobile phase consisting of ammonium acetate （0.5 mmol/L） and acetonitrile （10： 90, v/v） without on-line post-column oxidation with PbO2 which had been widely used in the previous methods. Identification and quantification were performed using multiple reaction monitoring （MRM） with one precursor ion, and two product ions for each analyte and electrospray ionization in positive mode. The limits of detection were 0.5 ng/g. The recoveries were in the range of 77.6% -98. 1%, and the relative standard deviations were less than 8.2%. The results showed that the method is suitable for the determination of residues of MG, LMG, CV and LCV in aquatic products.

关 键 词：液相色谱-串联质谱 孔雀石绿 结晶紫 隐色代谢物 水产品 

分 类 号：O658[理学—分析化学]