超高效液相色谱-串联质谱法同时检测水产品中 孔雀石绿、结晶紫及其代谢物的残留

Simultaneous determination of malachite green, crystal violet and their metabolites residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  孔雀石绿  结晶紫  超高效液相色谱-串联质谱法  水产品  基质效应

英文关键词:malachite green  crystal violet  ultra performance liquid chromatography-tandem mass spectrometry  aquatic product  matrix effect

中文摘要:

      目的 建立同时检测水产品中孔雀石绿(malachite green, MG)、隐色孔雀石绿(leucomalachite green, LMG)、结晶紫(crystal violet, CV)和隐色结晶紫(leucocrystal violet, LCV)等残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)的分析方法。方法 样品经乙腈提取, 经中性氧化铝柱净化, 采用超高效液相色谱-串联质谱法以电喷雾正离子化模式(electrospray ionization, ESI+)和多反应监测(multiple reaction monitoring, MRM)扫描模式进行测定, 以同位素内标法定量。同时考察了基质效应对检测结果的影响。结果 水产品中MG、LMG、CV和LCV的基质效应不同, 其中LCV的基质效应最为明显, 加标回收率较低(约50%)。MG、LMG、CV和LCV 4种物质在0.2~5.0 ng/mL浓度范围内呈良好线性, 相关系数均大于0.999, 方法检出限为0.1~0.2 μg/kg。MG、LMG和CV的加标回收率为93.5%~109.2%, 相对标准偏差为5.4%~9.6% (n=6)。结论 该方法仪器分析时间短、定量准确、检出限低, 可用于检测水产品中MG、LMG、CV和LCV的残留量。

英文摘要:

      Objective To establish a method for simultaneous determination of malachite green (MG), leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with acetonitrile, cleaned up with neutral alumina column, and then detected by UPLC-MS/MS with electrospray ionization (ESI+) mode and multiple reaction monitoring (MRM) mode. Isotope internal standards were used for quantification. Meanwhile the matrix effects were also observed. Results Different matrix effects existed in 4 kinds of analytes, especially in the LCV. The recovery of LCV was low (about 50%). MG, LMG, CV, and LCV had good linear relationships in the range of 0.2~5.0 ng/mL (r>0.999). The limits of detection (LOD) were 0.1~0.2 μg/kg. The recoveries of MG, LMG and CV were ranged from 93.5% to 109.2% . The relative standard deviations (RSDs) were 5.4%~9.6% (n=6). Conclusion The method is rapid, accurate and sensitive, which is suitable for the detection of MG, LMG, CV and LCV residues in aquatic products.