【作者】 刘桂华； 刘红河；

【Author】 LIU Gui-hua LIU Hong-he,Shenzhen Center for Disease Control and Prevention,Shenzhen 518020,China

【机构】 深圳市疾病预防控制中心；

【摘要】 目的建立测定水中孔雀石绿及其代谢物隐性孔雀石绿的同位素内标稀释高效液相色谱一串联质谱法。方法水样中加入氘代同位素内标,经 SCX 提取净化后,MRM 定量。结果方法的线性范围为0.2～5μg/L,孔雀石绿和隐色孔雀石绿的线性相关系数分别为0.9993和0.9991, 检出限均为0.001ng/L。在0.2、5、10 ng/100mL 三个浓度水平加标回收率为93.6%～107.5%, RSD 为3.7%～9.3%。结论该方法高效、灵敏、特异性强,准确度、精密度好,满足水样准确定性、定量要求,为孔雀石绿的溯源调查和卫生监督提供科学依据。更多还原

【Abstract】 Objective A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed to quantitate and confirm the presence of malachite green and leucomalachite green in water by using isotope internal standard dilution technique.Methods Sample was spiked with deuterium labeled isotope internal standards,extracted and cleaned by SPE of SCX column. Quantitative results were based on MRM.Results The calibration curve of malachite green and leucomalachite green showed good linearity in the range of 0.2～5 μg/L with correlation coefficient of 0.9993 and 0.9991 respectively.The detection limits of the method were 0.001 ng/L for both malachite green and leucomalachite green.The average recoveries at three levels(0.2、5、10 ng/kg) ranged from 93.6%～107.5% with RSD from 3.7% to 9.3%.Conclusion The method can identify and quantify malachite green and its metabolite leucomalachite green in fish pond water with satisfactory sensitivity,accurate and precision.更多还原