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首页> 外文期刊>Food Control >Simultaneous determination of malachite green, gentian violet and their leuco-metabolites in shrimp and salmon by liquid chromatography-tandem mass spectrometry with accelerated solvent extraction and auto solid-phase clean-up.
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Simultaneous determination of malachite green, gentian violet and their leuco-metabolites in shrimp and salmon by liquid chromatography-tandem mass spectrometry with accelerated solvent extraction and auto solid-phase clean-up.

机译：液相色谱-串联质谱-加速溶剂萃取-自动固相净化-同时测定虾和鲑鱼中的孔雀石绿，龙胆紫及其隐色代谢产物。

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摘要

An automated method had been developed for the determination of Malachite green and Gentian violet as well as their leuco-metabolites in shrimp and salmon by liquid chromatography-tandem mass spectrometry with accelerated solvent extraction and auto solid-phase clean-up. The target analytes were extracted using accelerated solvent extraction (ASE) and then purified using auto solid-phase clean-up. The ASE conditions as: solvent, temperature, pressure, static time, and cell size were optimized. The optimum extraction conditions were set as the following aspects: using 22 mL ASE cell, McIlvaine buffer (pH 3)/acetonitrile/hexane (2/10/2, v/v) as the extraction solvent; pressure at 1500 psi; temperature at 60 degrees C; static time 5 min (static time); one cycles. The extracts were purified on OASIS MCX SPE column. Detection and quantification of Malachite green; gentian violet; leucomalachite green; leucogentian violet were performed by reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC-ESI-MS/MS). An averaged decision limits (CC alpha) and detection capability (CC beta) of the method were in the range of 0.005 mug/kg {unknown symbol} 0.012 mug/kg and 0.08 mug/kg {unknown symbol} 0.13 mug/kg in shrimp and salmon. The recoveries of Malachite green; Gentian violet; Leucomalachite green; Leucogentian violet at levels of 0.1-1.0 mug/kg averaged from 82.1 to 102.9% with the relative standard derivation less than 14.6%. This method is precise, sensitive and highly efficient in extraction. What's more, after routine applications, it's turned out that this method is suitable for the determination of Malachite green, Gentian violet and their leuco-metabolites in shrimp and salmon.
机译：通过液相色谱-串联质谱，加速溶剂萃取和自动固相净化，开发了一种自动方法，用于测定虾和鲑鱼中的孔雀石绿和龙胆紫以及它们的无色代谢产物。使用加速溶剂萃取（ASE）萃取目标分析物，然后使用自动固相净化法纯化。优化了ASE条件，例如：溶剂，温度，压力，静态时间和像元大小。最佳提取条件设定为以下几个方面：使用22 mL ASE细胞，McIlvaine缓冲液（pH 3）/乙腈/己烷（2/10/2，v / v）作为提取溶剂;压力为1500 psi;温度在60摄氏度;静态时间5分钟（静态时间）;一个周期。将提取物在OASIS MCX SPE柱上纯化。孔雀石绿的检测和定量;龙胆紫白孔雀石绿;通过反相液相色谱结合电喷雾电离三重四极杆质谱（LC-ESI-MS / MS）进行亮光紫。该方法的平均决策极限（CC alpha）和检测能力（CC beta）在虾的0.005马克/千克{未知符号} 0.012马克/千克和0.08马克/千克{未知符号} 0.13马克/千克的范围内和三文鱼。孔雀石绿的回收率;龙胆紫白孔雀石绿; 0.1-1.0杯/千克的亮白紫罗兰平均含量为82.1％至102.9％，相对标准偏差小于14.6％。该方法精确，灵敏且提取效率高。而且，在常规应用之后，事实证明该方法适用于虾和鲑鱼中孔雀石绿，龙胆紫及其隐色代谢产物的测定。

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