孔雀石绿等染料物质残留检测过程中实验室污染的来源分析

Analysis of Pollution Sources in Laboratory During the Determination of Residual Dyes Such as Malachite Green

关键词:  超高效液相色谱-串联质谱法  孔雀石绿  结晶紫  亚甲基蓝  残留检测

Key words:  Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  Malachite green  Crystal violet  Methylene blue  Residual detection

摘要:

为了分析孔雀石绿等残留检测过程中实验室污染的来源，本研究应用超高效液相-串联质谱联用法（UPLC-MS/MS）测定了常用实验室用品中孔雀石绿、无色孔雀石绿、结晶紫、无色结晶紫、亚甲基蓝的含量。纸样品用乙腈直接提取；笔样品采用书写痕迹后再用乙腈提取，UPLC-MS/MS定量测定。结果表明：在纸样品中，除了实验滤纸外，其它纸样品（如A4打印纸、报纸、标签纸等）均含有一定水平的目标物量；笔样品中，除了铅笔2H、中性笔135012蓝、中性笔2180蓝色外，其它笔样品（如圆珠笔、记号笔、签字笔、水笔等）含有一定水平的目标物量。为了降低实验室目标物污染风险，本文还对样品处理前和处理中的各个环节需要注意的问题做了较为详细的讨论。本研究结果将有利于建立有效预防体系从而尽量避免样品在该类物质残留检测中的实验室本底污染和假阳性结果。

Abstract:

To analyze the pollution sources in laboratory during the determination of residues such as malachite green, an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was used to determine the contents of malachite green (MG), leucomalachite green (LMG), crystal violet (CV), leucocrystal violet (LCV), and methylene blue (MB) in common laboratory paraphernalias. The paper samples were extracted by acetonitrile, and for pen samples the marks written by pen was extracted by acetonitrile. UPLC-MS/MS was used for quantitative analysis. Results showed that as to paper samples, certain contents of the above objects were found in A4 printing paper, newspaper, and labeled paper, but not in experimental filter paper. For pen sample, certain contents of the above five objectives were found for ball-point pen, marker pen, signing pen and bosh, but not for pencil (2H), neutral pen (135012 blue), neutral pen (2180 blue). Furthermore, the problems that should be paid attention in the each procedure prior to and in the sample treatment were discussed in detail to reduce the risk of objects pollution in laboratory. The results of the present study would be beneficial to develop effective guard system for the prevention of background pollution in lab and false positive results as much as possible during the detection of the residual above objects.