高效液相色谱-串联质谱法测定鲜海参中的孔雀石绿及代谢物  

Determination of malachite green and metabolites residues in fresh sea cucumber by high performance liquid chromatography-tandem mass spectrometry

作　　者：郭晓艳 王猛 单晓辉 李东浩 刘鑫 

机构地区：[1]龙口出入境检验检疫局,龙口265700 [2]莱州出入境检验检疫局,莱州261400 [3]黄岛出入境检验检疫局,黄岛266000

出　　处：《食品安全质量检测学报》2017年第11期4184-4189,共6页Journal of Food Safety and Quality

摘　　要：目的建立测定鲜海参中孔雀石绿及代谢物的高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)。方法本文对行业标准GB/T 19857-2005《水产品中孔雀石绿和结晶紫残留量的测定》的前处理方法进行了改进,针对海参样品粘稠、蛋白质含量高的特点,以氘代孔雀石绿、氘代无色孔雀石绿分别为孔雀石绿、无色孔雀石绿的同位素内标进行定量,高效液相色谱-串联质谱仪检测。结果孔雀石绿及无色孔雀石绿在0.5~10.0μg/kg质量浓度范围内线性关系良好(R2>0.999),在0.5、1.0、1.5μg/kg 3个质量浓度水平添加,平均回收率为85.0%~105.0%,相对标准偏差均小于1.4%。结论本研究建立的方法适合于鲜海参中孔雀石绿及代谢物的检测。Objective To establish a method for determination of malachite green and metabolites residues in fresh sea cucumber by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Methods The pre-treatment method of industry standard（GB/T 19857-2005 Determination of malachite green and crystal violet residues in aquatic product） was improved. According to the characteristics of stickiness and high protein content of sea cucumber sample, the isotopic internal standard of malachite green and leucomalachite green was separately measured quantitatively with deuterated malachite green and deuterated leucomalachite green and detected by HPLC-MS/MS. Results Malachite green and leucomalachite green had good linear relationships in the concentration of 0.5-10.0 μg/kg（R^2〉0.999）. The average recovery rates were 85%-105% at the spiked levels of 0.5, 1.0 and 1.5 μg/kg and the relative standard deviations were less than 1.4%. Conclusion The established method is suitable for detection of malachite green and metabolites residues in fresh sea cucumber.

关 键 词：鲜海参 高效液相色谱-串联质谱法 孔雀石绿 无色孔雀石绿 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]