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| 超高效液相色谱-串联质谱法快速测定鱼类中孔雀石绿、结晶紫及其隐色代谢物 |
| Rapid determination of the residues of malachite green, crystal violet and their leuco metabolites in fish by ultra perfprmance liquid chromatopraphy-tandem mass spectrometry |
| 投稿时间：2025-02-19 修订日期：2025-06-23 |
| DOI： |
| 中文关键词: 超高效液相色谱-串联质谱法,孔雀石绿,结晶紫,隐色孔雀石绿,隐色结晶紫,鱼类 |
| 英文关键词:ultra performance liquid chromatography tandem mass spectrometry malachite green, crystal violet leucomalachite green leucocrystal violet, fish. |
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| 中文摘要: |
| 目的 建立固相萃取技术（solid phase extraction, SPE）结合超高效液相色谱串联质谱（ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS）测定鱼类中孔雀石绿、结晶紫、隐色孔雀石绿、隐色结晶紫的测定方法。方法 样品经乙腈沉淀蛋白并萃取后，过HMR-Lipid SPE柱通过式净化。以乙腈和乙酸铵溶液为流动相梯度洗脱，采用BEH shield C18色谱柱分离，ESI源正离子模式进行多反应监测（multiple reaction monitoring, MRM）扫描，内标法定量。结果 4种目标化合物的线性范围在0.20～10.0 ng/mL，相关系数（r）＞0.999，检出限为0.05 μg/kg。3个加标水平下（2、5、10 μg/kg）的回收率为80.1%～105.2%，相对标准偏差为1.2%～14.3%。结论 本方法灵敏、快速、准确，适用于于鱼类中孔雀石绿、结晶紫及其的隐色代谢物的检测，可为鱼类的质量检测及市场监管提供技术支撑。 |
| 英文摘要: |
| Objective To establish a sensitive and rapid method for the determination of malachite green, crystal violet, leucomalachite green and leucocrystal violet in fish by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods The target analytes were extracted from fish with acetonitrile, followed by purified by solid phase extraction column named HMR-Lipid. The analytes were then separated by the BEH shield C18 chromarographic column using a mobile phase gradient with acetonitrile and ammonium acetate. The positive ion mode of the ESI source was used for multiple reaction monitoring scanning, and the internal standard method was used for quantification. Results The linear ranges of the four target analytes were 0.2~10 ng/mL, with correlation coefficient(r)﹥0.999. The limit of detection(LOD)within 0.05 μg/kg. The recoveries at three spiking levels（2, 5, 10 μg/kg） were 80.1%~105.2%, and the relative standard deviations (RSD) were 1.2%~14.3%. Conclusion The method is rapid, sensitive and accurate, and is suitable for the determination of malachite green, crystal violet and their leuco metabolites in fish. It can provide support for quality control and market supervision. |
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