论文部分内容阅读
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 performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was developed for the simultaneous determination of malachite green, crystal violet and its metabolites (tactile malachite green and leuco crystal violet) in aquaculture water and sediments Analytical method. The samples were vacuum freeze-dried, extracted with acetonitrile and dichloromethane and cleaned up by MCX solid-phase extraction cartridges. The samples of aquaculture water were vacuum freeze-dried and dissolved in 50% acetonitrile-water with 0.1% formic acid. Detection. Separation by BEH C18 column, gradient elution, multiple reaction monitoring positive mode quantitative and qualitative analysis. The internal standard method was used for quantification. The linear range was 0.50 ~ 50μg / L and the correlation coefficient was greater than 0.99. The detection limit and limit of quantification of aquaculture water were 10-25 ng / L and 25 ~ 50 ng / L. The detection limits and the limits of quantitation of sediment were 0.020-0.025 μg / kg and 0.04-0.05 μg / kg respectively. The average recoveries were 85.2% -105.6% with relative standard deviations less than 12%. The method has been applied to the determination of illicit drugs in actual aquaculture and sediment samples.