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首页> 外文期刊>Journal of Chromatographic Science >Simultaneous determination of malachite green, crystal violet, methylene blue and the metabolite residues in aquatic products by ultra-performance liquid chromatography with electrospray ionization tandem mass spectrometry
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Simultaneous determination of malachite green, crystal violet, methylene blue and the metabolite residues in aquatic products by ultra-performance liquid chromatography with electrospray ionization tandem mass spectrometry

机译:超高效液相色谱-电喷雾电离串联质谱法同时测定水产品中的孔雀石绿,结晶紫,亚甲基蓝和代谢物残留

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This work describes solid-phase extraction-ultra-performance liquid chromatography with electrospray ionization tandem spectrometry for determination of malachite green and metabolite leucomalachite green, crystal violet and metabolite leucocrystal violet, methylene blue and metabolites including azure A, azure B and azure C in aquatic products. Samples were extracted with acetonitrile and ammonium acetate buffer and purified by liquid extraction with dichloromethane, and then on MCAX solid-phase extraction cartridges. Then the extract was evaporated at 458C by nitrogen blow. The residue was dissolved and separated by an Acquity BEH C18 column. The mobile phase was acetonitrile (A) and 5 mmol/L of ammonium acetate containing 0.1% formic acid (B). Analytes were confirmed and quantified using a tandem mass spectrometry system in multiple reaction mode with triple quadrupole analyzer using positive polarity mode. The limits of detection of malachite green, leucomalachite green, crystal violet and leucocrystal violet were 0.15 μg/kg, the limits of quantification were 0.50 μg/kg, and the average recoveries were more than 75% with spiked residues from 0.5 to 10 μg/kg. The relative standard deviations were less than 13%. The limits of detection of methylene blue, azure A, azure B and azure C were 0.3 μg/kg, the limits of quantification were 1.0 μg/kg, the average recoveries were more than 70% with spiked residues from 1.0 to 10 μg/kg and the relative standard deviations were less than 15%. The method has the merits of simplicity, sensitivity and rapidity, and can be used for simultaneous determination of the analytes in aquatic products.
机译:这项工作描述了固相萃取-超高效液相色谱-电喷雾电离串联质谱法测定水中的孔雀石绿和代谢产物白孔雀绿,结晶紫和代谢产物无色结晶紫,亚甲基蓝和代谢产物,包括水中的天蓝色A,天蓝色B和天蓝色C产品。样品用乙腈和乙酸铵缓冲液萃取,并用二氯甲烷进行液体萃取,然后在MCAX固相萃取柱上纯化。然后通过氮气吹扫将提取物在458℃蒸发。将残余物溶解并通过Acquity BEH C18柱分离。流动相为乙腈(A)和5 mmol / L含0.1%甲酸(B)的乙酸铵。使用串联质谱系统在多重反应模式下使用正极模式的三重四极杆分析仪对分析物进行确认和定量。孔雀石绿,孔雀石绿,结晶紫和无色结晶紫的检出限为0.15μg/ kg,定量限为0.50μg/ kg,平均回收率超过75%,加标残留量为0.5至10μg/ kg公斤。相对标准偏差小于13%。亚甲基蓝,天蓝色A,天蓝色B和天蓝色C的检出限为0.3μg/ kg,定量限为1.0μg/ kg,平均回收率超过70%,残留物浓度为1.0至10μg/ kg相对标准偏差小于15%。该方法具有简便,灵敏,快速的优点,可用于同时测定水产品中的分析物。

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