超高效液相色谱-串联质谱法测定养殖水和沉积物中孔雀石绿、结晶紫及其代谢物残留  

Determination of malachite green,crystal violet and its metabolites residues in aquaculture water and sediment using ultra-high performance liquid chromatography tandem mass spectrometry

作　　者：王旭峰[1] 王强[1] 赵东豪[1] 黄珂[1] 黎智广[1] 李永贤[1] 杨宏亮[1] 李刘冬[1] 

机构地区：[1]中国水产科学研究院南海水产研究所,农业部水产品加工重点实验室,农业部水产品贮藏保鲜质量安全风险评估实验室(广州),农业部渔业环境及水产品质量监督检验测试中心(广州),广州510300

出　　处：《分析试验室》2015年第6期702-706,共5页Chinese Journal of Analysis Laboratory

基　　金：中央级公益性科研院所基本科研业务项目费专项资金项目(2014TS09;2014TS10;2013TS08);国家农产品质量安全风险评估重大专项(GJFP2014009)资助

摘　　要：建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定养殖水和沉积物中孔雀石绿、结晶紫及其代谢物（隐性孔雀石绿和隐色结晶紫）的多残留分析方法。沉积物样品真空冷冻干燥,乙腈和二氯甲烷提取,MCX固相萃取小柱净化;养殖水试样真空冷冻干燥,50%乙腈-水溶液（含0.1%甲酸）溶解残渣,离心过膜,上机检测。经BEH C18色谱柱分离,梯度洗脱,多反应监测正离子模式下进行定量和定性分析。采用内标法定量,药物含量在0.50~50μg/L范围内线性关系良好,相关系数大于0.99;以3倍和10倍信噪比计算出养殖水的检测限和定量限为10~25 ng/L和25~50 ng/L,沉积物的检测限和定量限为0.020~0.025μg/kg和0.04~0.05μg/kg;平均回收率为85.2%~105.6%,相对标准偏差小于12%。方法已用于实际养殖水和沉积物样品中违禁药物的测定。An ultra high performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS） method was developed for the simultaneous determination of malachite green （MG）, crystal violet （CV）, and its metabolites （leucomalachite green （LMG） and leucocrystal violet （LCV）） residues in aquaculture water and sediment. Sediment samples were freeze-dried under vacuum and extracted with acetonitrile and dichloromethane, followed by cleanup using MCX solid phase extraction cartridge; the freeze-dried residues of aquaculture water were reconstructed in 50% acetonitrile-water solution （containing 0. 1 % formic acid） and then centrifuged anti filtered before UPLC-MS/MS analysis. Chromatography separation was accomplished ona Waters BEH C18column under gradient elution condition. Qualitative and quantitative analysis of target analytes was carried out in multiple reaction monitor （MRM） positive ionization mode. Internal standard calibration curves were obtained in the concentration range of 0. 50 -50 μg/L with good correlation coefficients （r 〉 0. 99）. The limits of detection （LODs） and the limits of quantification （LOQs） were in the range of l0 - 25 ng/L （ S/N= 3 ） and 25 - 50 ng/L （S/N = 10） for aquaculture water, while 0. 020 - 0. 025 μg/kg and 0. 04 - 0. 05 μg/kg for sedment respectively. The mean recoveries were between 85.2% and 105.6% with relative standard deviation （RSD） less than 12%. The proposed method was applied to the determination of prohibited drugs in real aquaculture water and sediment samples, which obtained satisfactory results.

关 键 词：超高效液相色谱-串联质谱 残留分析 养殖水 沉积物 

分 类 号：O657.63[理学—分析化学]