同位素稀释质谱法测定三文鱼中的孔雀石绿  

Confirmatory Analysis of Malachite Green by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

作　　者：汤桦[1] 陈大舟[1] 张庆合[1] 于慧梅[2] 徐锐锋[1] 

机构地区：[1]中国计量科学研究院,北京100013 [2]北京化工大学,北京100013

出　　处：《化学通报》2008年第6期408-414,共7页Chemistry

基　　金：国家科技基础条件平台项目(2005DKA10804)资助

摘　　要：建立了三文鱼中孔雀石绿和无色孔雀石绿的同位素稀释质谱测定法，即：通过添加作为同位素稀释剂的氘代孔雀石绿和无色孔雀石绿到样品中，经液液萃取、提取液中添加中性氧化铝以及过碱性氧化铝小柱进行净化的前处理，然后由以乙腈和乙酸铵缓冲液（0．05mol／L，pH 4．5）为流动相的液相色谱／离子阱质谱联用来作为分离检测手段。对含不同浓度孔雀石绿和无色孔雀石绿的储备液在不同溶剂、酸度、时间和温度的稳定性、前处理过程中的中性氧化铝的合适添加量、破乳剂的选择、孔雀石绿和无色孔雀石绿在氮吹和旋蒸过程中的损失以及液相色谱和质谱条件进行了研究。该方法的孔雀石绿和无色孔雀石绿的回收率分别为95．6％～103．3％和97．64％～100．80％，检测限为0．4和0．3μg／kg，相对标准偏差分别为4．76％～6．13％和3．14％～5．67％。结果表明，所建立的方法快速、灵敏、准确、可靠。A quantitative liquid chromatography--tandem mass spectrometric （LC--MS/MS） method has been developed for the determination of malachite green （MG） and its metabolite leucomalachite green （LMG） in salmon fish. Residues were extracted with the acetonitrile-acetate system. The samples were purified by using neutral alumina in extraction process and alkaline alumina SPE column, then it was analyzed with a reversed-phase LC-MS/MS using a positiveion electrospray ionisation （ ESI）. Isotope-labelled malachite green （ MG-D5 ） and leucomalachite green （ LMG-D5 ） were used as an internal standard for the quantification of MG and LMG residues. The detection limit for MG and LMG was 0.4 and 0.3 μg/kg, respectively.The relative recovery was in the range of 95.6% - 103.3% for MG and 97.64% - 100.80% for LMG. The stability of MG and LMG stock solutions was studied in different conditions, such as solvent, acidity, time and temperature. The loss of MG and LMG in the process of nitrogen blowing and vacuum evaporation was investigated.

关 键 词：同位素稀释质谱法 孔雀石绿 无色孔雀石绿 三文鱼 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]