液质联用法测定水产品中孔雀石绿和隐色孔雀石绿残留量
目的 建立一种高效液相色谱法-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定水产品中孔雀石绿和隐色孔雀石绿残留量的分析方法。方法 分析采用Shiseido C18色谱柱(2.0 mm×150 mm, 5 μm), 流动相A为乙腈, 流动相B为5 mmol/L乙酸铵(pH=4.5), 流动相比例A:B=75:25(V:V), 等度洗脱。流速: 0.2 mL/min, 柱温: 35 ℃, 采用电喷雾离子源正离子扫描(electron spray ionization, ESI+), 多反应监测模式对样品进行检测(multiple reaction monitoring, MRM)。结果 孔雀石绿在1.152~23.04 ng/mL浓度范围内线性良好, 相关系数r为0.999; 隐色孔雀石绿在1.216~24.32 ng/mL浓度范围内线性良好, 相关系数r为0.999。本方法回收率范围在89.1%~105.7%, 精密度在2.9%~3.9%。检出限为 0.2 μg/kg。结论 该方法前处理简单快捷, 灵敏度高, 检测成本降低, 结果准确可靠, 可适用于水产品中孔雀石绿和隐色孔雀石绿的测定。
Objective To establish a method for the determination of malachite green and leucomalachite green residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Shiseido C18 column(2.0 mm×150 mm, 5 μm) was used for analysis. Isocratic elution was performed with acetonitrile as mobile phase A, 5 mmol/L ammonium acetate (pH=4.5) as mobile phase B, mobile phase A:B=75:25(V:V), and mobile phase flow rate was 0.2 mL/min, column temperature was 35 ℃. The samples were detected by electron spray ionization(ESI+) and multiple reaction monitoring (MRM). Results The relationship between logarithmic peak area and logarithmic of malachite green concentration showed good linear over the range of 1.15223.04 ng/mL, with a correlation coefficient (r) of 0.999. The relationship between logarithmic peak area and logarithmic of leucomalachite green concentration showed good linear over the range of 1.21624.32 ng/mL, with a correlation coefficient (r) of 0.999. The average recoveries of the method were between 89.1%105.7%, and the precision was between 2.9%3.9%. The detection limit was 0.5 μg/kg. Conclusion This method is simple sampling preparation, rapid, sensitive, low detection cost and accurate, which is effective and suitable for the detection of MG and LMG in aquatic products.
标题：液质联用法测定水产品中孔雀石绿和隐色孔雀石绿残留量
英文标题：Determination of malachite green and leucomalachite green residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry
作者：
王蓓蓓 西安市食品药品检验所
李尔春 西安市食品药品检验所
卫星华 西安市食品药品检验所
李敏 西安市食品药品检验所
张亚锋 西安市食品药品检验所
中文关键词:高效液相色谱-串联质谱法,水产品,孔雀石绿,隐性孔雀石绿,
英文关键词:high performance liquid chromatography-tandem mass spectrometry,aquatic products,malachite green,leucomalachite green,
发表日期：2020-01-20
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