渔业养殖水体中孔雀石绿、结晶紫及其代谢物残留量的检测方法研究  

Determination of malachite green, crystal violet and their metabolites in aquaculture water

作　　者：杨盈悦 朱羽庄 梅光明[2,3] 李晋成 YANG Yingyue;ZHU Yuzhuang;MEI Guangming;LI Jincheng(College of Food and Pharmaceutial Sciences of Zhejiang Ocean University,Zhoushan 316021,Zhejiang Province,China;Marine Fisheries Research Institute of Zhejiang,Zhoushan 316021,Zhejiang Province,China;Zhejiang Key Laboratory of Marine Aquaculture,Zhoushan 316021,Zhejiang Province,China;Chinese Academy of Fishery Sciences,Beijing 100141,China)

机构地区：[1]浙江海洋大学食品与药学学院,浙江舟山316021 [2]浙江省海洋水产研究所,浙江舟山316021 [3]浙江省海水增养殖重点实验室,浙江舟山316021 [4]中国水产科学研究院,北京100141

出　　处：《浙江大学学报（理学版）》2021年第4期461-469,共9页Journal of Zhejiang University（Science Edition）

基　　金：浙江省科技计划项目(LGN20C200015)。

摘　　要：建立了渔业养殖水体中孔雀石绿、结晶紫及其代谢物残留量的检测方法。水样经二氯甲烷液液萃取、中性氧化铝填料吸附除杂后,采用超高效液相色谱-串联质谱法检测。色谱条件为:Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),柱温40℃,流动相由5 mmol·L^(-1)的乙酸铵缓冲溶液(含0.1%甲酸)和乙腈组成,梯度洗脱程序,流速为0.3 mL·min^(-1)。质谱条件为:电喷雾正离子模式、多反应监测扫描模式、内标法。结果表明,在标准溶液浓度为0.2~5.0μg·L^(-1)时,孔雀石绿、隐色孔雀石绿、结晶紫和隐色结晶紫4种组分的质谱信号强度与浓度之间均呈较好的线性关系,相关系数r大于0.998,方法检测限和定量限分别为2 ng·L^(-1)和5 ng·L^(-1)。在空白水样为5~100 ng·L^(-1)的添加浓度梯度下,4种组分的平均加标回收率为81.8%~109.5%,批内精密度和批间精密度均小于10%。说明该方法准确率高、重现性好,且定量限低,能满足对渔业养殖水体中孔雀石绿、结晶紫及其代谢物残留量的检测要求。A method for the determination of malachite green,crystal violet and their metabolites in aquaculture water was established.The samples were prepared using dichloromethane liquid-liquid extraction followed by cleanup of neutral alumina filler adsorption.Acquity UPLC BEH C18 column(2.1 mm×100 mm,1.7μm),mobile phase composed of 5 mmol·L^(-1) ammonium acetate buffer solution(contain 0.1%formic acid)and acetonitrile and flow rate of 0.3 mL·min^(-1) were assumed for the chromatography separation at 40℃.Electrospray ion source positive ion scanning,multi-reaction monitoring mode and internal standard method were conducted to analyze and quantify the target objects.The results showed that within the standard solution concentration ranges of 0.2-5.0μg·L^(-1),there existed a good linear relationship between the signal strength and concentrations of 4 target objects(correlation coefficient r were all above0.998).The limits of detection and limits of quantitative were 2 and 5 ng·L^(-1),respectively.Spiked with gradient concentrations of 5-100 ng·L^(-1) in the blank water sample,the recovery rates of the four components were 81.8%-109.5%,and the in-batch precision and inter-batch precision were both less than 10%.It showed that the method had the advantage of high accuracy,good reproducibility and quantitative limit,and could meet the requirements of trace detection of malachite green,crystal violet and their metabolites in aquaculture water.

关 键 词：养殖水体 孔雀石绿 结晶紫 代谢物残留 超高效液相色谱-串联质谱法 

分 类 号：X832[环境科学与工程—环境工程] S949[农业科学—水产养殖]