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

Determination of malachite green and leucomalachite green residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

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

中文摘要:

      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。

英文摘要:

      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.