Rapid Determination of Residual Amounts of Malachite Green and Leuco Malachite Green in Aquatic Products by Ultra-High Performance Liquid Chromatography in Hyphenation with Tandem Mass Spectrometry
摘 要
采用超高效液相色谱(UHPLC)与串联质谱(MS/MS)联用对水产品中残留量的孔雀石绿(MG)及无色孔雀石绿(LMG)进行了快速检测.经均匀化处理的试样用乙腈在pH 4.5的乙酸盐缓冲介质中萃取使MG及LMG萃入有机相,所得萃取液用液-液分配,先后用酸性氧化铝及氯化钠和酸性氧化铝及无水硫酸钠进行分离及净化.上层清液经0.2 μm滤膜过滤后供UHPLC-MS/MS分析,采用电喷雾离子化(ESI+)及多反应监测模式进行测定,用D5-MG及D6-LMG内标法进行定量.在优化的试验条件下,使质谱分析中的基体效应得到合理降低.方法的测定下限(S/N=10),MG为0.19 μg·kg-1,LMG为0.10 μg·kg-1,在0.5~5.0 μg·kg-1浓度范围内作标准加入法,方法的回收率在89.4%~110%范围内.相对标准偏差(n=6)值在5.9%~9.8%.
Abstract
Residual amounts of malachite green (MG) and leuco malachite green (LMG) in aquatic products were determined by ultra-high performance liquid chromatography (UHPLC) hyphenated with tandem mass spectrometry (MS/MS).The compounds,MG and LMG,were extracted from the homogenized tissue sample with acetonitrile in an acetate buffer medium of pH 4.5,separated and purified by liquid-liquid partition and acidic alumina and sodium chloride,as well as acidic alumina and anhydrous sodium sulfate in succession.The clear supernatant liquid after fitration with 0.2 μm filtering membrane was ready for UHPLC-MS/MS analysis.Determinations were performed by using electrospray ionization (ESI+) and multi-reaction monitoring (MRM) modes.Internal standards of D5-MG and D6-LMG were used in the quantification.Under optimized conditions of sample pretreatment and operation of instruments,matrix effect on the MS determination was reduced rationally.Determination (S/N=10) for MG and LMG were found to be 0.19 and 0.10 μg·kg-1 respectively.Tests for recovery were made by addition of standards in the concentration range of 0.5 to 5.0 μg·kg-1,and results obtained were ranged from 89.4% to 110%.Values of RSD′s (n=6) were found in the range of 5.9%-9.8%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2007/3/25
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备注苏建峰(1979-),男,福建福州人,硕士,主要从事食品中污染物残留检测.
引用该论文: SU Jian-feng,LIAN Wen-hao,CHEN Wen-kai. Rapid Determination of Residual Amounts of Malachite Green and Leuco Malachite Green in Aquatic Products by Ultra-High Performance Liquid Chromatography in Hyphenation with Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(11): 937~939
苏建峰,连文浩,陈文凯. 孔雀石绿及无色孔雀石绿[J]. 理化检验-化学分册, 2007, 43(11): 937~939
被引情况:
【1】赵善贞,周瑶,盛永刚,张旖,谌鸿超,邓晓军, "高效液相色谱-四极杆串联线性离子阱质谱法测定水产品及饲料中的孔雀石绿、结晶紫及其代谢物",理化检验-化学分册 50, 35-39(2014)
【2】侯建波,谢文,祝泽龙,曾淦宁,吕春华,何建敏, "液相色谱-串联质谱法同时测定水产品中三苯甲烷类与噻嗪类染料及其代谢产物",理化检验-化学分册 51, 403-408(2015)
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参考文献
【1】GB/T 19857-2005水产品中孔雀石绿和结晶紫残留量的测定[S].
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【3】谢文,丁慧瑛,奚君阳,等.水产品中孔雀石绿、结晶紫及其代谢产物残留量的检测[J].色谱,2006,24(5):529-530.
【4】安蓉,薄美萍.超高效液相色谱(UPLCTM)与质谱联用技术:改善药残和代谢物分析的结果质量[J].现代科学仪器,2006(1):20-24.
【5】瞿进文,吴洁珊,蔡勤仁,等.液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量[J].理化检验-化学分册,2005,41(11):799-801.
【6】Matuszewski B K,Constanzer M L,Chavez-Eng C M.Matrix effect in quantitative LC/MS/MS analyses of biological fluids:a method for determination of finasteride in human plasma at picogram per milliliter concentrations[J].Anal Chem,1998,70(5):882-889.
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