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当前位置: 首页 > 文章 > 超高效液相色谱一串联质谱法测定水产苗种中孔雀石绿及其代谢物隐色孔雀石绿 食品科学 2013,34 (12) 171-177
Position: Home > Articles > Determination of Malachite Green and Its Metabolite Leucomalachite Green in Aquatic Fingerlings by Ultra  Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-ESI-MS/MS) FOOD SCIENCE 2013,34 (12) 171-177

超高效液相色谱一串联质谱法测定水产苗种中孔雀石绿及其代谢物隐色孔雀石绿

作  者：
田秀慧;于召强;陈玮;任传博;邹荣婕;张华威
单  位：
关键词：
水产;苗种;孔雀石绿;隐色孔雀石绿;超高效液相色谱;串联质谱法;代谢物
摘  要：
建立水产苗种中孔雀石绿及其代谢物隐色孔雀石绿的超高效液相色谱-串联质谱检测方法,内标法定量.样品用乙腈提取后,以乙腈定容至25.0mL,取5.0mL上述样品溶液经中性氧化铝柱净化,收集全部流出液,45℃氮吹至将尽干,准确加入2.00mL乙腈-5mmol/L的乙酸铵溶液(1:1,纠功定容,超声振荡1min,样液经0.22μm滤膜,在ACQUITYTMUPLCBEHC18(1.7gm,2.1mmi.d.*100mm)色谱柱上进行梯度洗脱分离;流动相为乙腈和含有0.1%甲酸的5mmol/L的乙酸铵溶液;多反应监测模式下用超高效液相色谱.串联质谱测定其中孔雀石绿及其代谢物残留量.本方法孔雀石绿和隐色孔雀石绿的线性范围为0.5~20.0ng/mL,相关系数为0.9991和O.9999;孔雀石绿和隐色孔雀石绿的检出限为0.03gg/kg,定量限为0.10gg/kg,在0.10、1.0μg/kg和2.0gg/kg三个水平加标平均回收率为84.3%~100.7%,相对标准偏差(RSD)为4.12%~9.18%.该方法灵敏度高,准确性好,相比较前人研究,在实验条件方面做出了一定的改进,适用于水产苗种中孔雀石绿和隐色孔雀石绿残留的测定.
译  名：
Determination of Malachite Green and Its Metabolite Leucomalachite Green in Aquatic Fingerlings by Ultra  Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-ESI-MS/MS)
关键词：
aquatic fingerlings%malachite green%leucomalachite green%ultra performance liquid chromatography tandem mass spectrometry%metabolite
摘  要：
A UPLC-ESI-MS/MS method was established for rapid determination of malachite green (MG) and its metabolite leucomalachite green (LMG) in aquatic fingerlings with quantification by isotope-labeled internal standard method. UPLC and MS/MS analytical conditions were examined and optimized by a series of experiments. Samples were extracted with acetonitrile, purified on a neutral Al2O3 solid phase extraction cartridge. All eluates were collected and blown to dryness under a nitrogen stream. The residue was re-dissolved in acetonitrile and ammonium acetate (1 + 1), sonficated and filtered prior to UPLC analysis. The mobile phase was composed of A (acetonitrile) and B (5 mmol/L of ammonium acetate containing 0.1% formic acid) at a flow rate of 0.25 mL/min. The analytes were finally detected and quantified using a triple Quadrapole MS/MS system in positive polarity multiple reaction mode. Malachite green and leucomalachite green showed good linearity over the range of 0.5 to 20.0 ng/mL with correlation coefficient of 0.9991 and 0.9999, respectively. The limits of detection of this method were 0.03 μg/kg for malachite green and leucomalachite green, and limits of quantification were 0.10 μg/kg. The average recoveries at three spiked levels (0.10, 1.0 μg/kg and 2.0 μg/kg) ranged from 84.3% to 100.7% with relative standard deviations from 4.12% to 9.18%. In addition, the method showed advantages of simplicity, sensitivity and accuracy, and could be applied for simultaneous determination of malachite green and leucomalachite green in aquatic fingerlings.

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