Chen Xinglian, Lin Tao, Liu Xingyong, Mei Wenquan, Yang Dongshun, Li Yangang, Li Maoxuan, Wang Luxiang
Quality Standardizing and Testing Technology Institute, Yunnan Academy of Agricultural Sciences, Kunming 650224, China.
Supervision & Testing Center for Farm Products Quality, Ministry of Rural Agriculture(Kunming Section), Kunming 650224, China.
Se Pu. 2019 Sep 8;37(9):946-954. doi: 10.3724/SP.J.1123.2019.02016.
A method was established to rapidly determine 20 kinds of veterinary drug residues including three catagories of antibiotics (sulfonamides, quinolones, and chloramphenicols) and two kinds of triphenylmethanes (malachite green (MG) and leucomalachite green (LMG)) in fish and shrimp, based on dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry. The samples were first hydrolyzed using a dipotassium hydrogen phosphate solution, and then extracted using acetonitrile. Afterward, the extraction solution was dehydrated and salted out with sodium chloride and condensed to nearly dry using a rotating evaporator. This residue was dissolved in 1.0 mL methanol. The resulting solution was purified by dispersive solid phase extraction method with C18 and PSA sorbents, and filtered through a filter. The target compounds were separated employing a ZORBAX C18 column. The mass spectrometer datas were acquired by multiple reaction monitoring (MRM) of positive and negative modes and quantitated applying the isotope internal standard method. The 20 veterinary drugs showed a good linear relationship in the range of 0.2-300 μg/L. The limits of detection and the limits of quantification were 0.1-0.6 and 0.3-1.8 μg/kg, respectively, while the correlation coefficients were greater than 0.99. The average recoveries at the three spiked levels (1, 5, and 20 times of quantitative limits) ranged between 72.5%-118%, with the relative standard deviations of 1.9%-9.8%. The advantages of method include a simple pretreatment, a high detection efficiency, and a low cost. Moreover, it is suitable for the simultaneous determination of multiple veterinary drug residues in fish and shrimp.
建立了一种基于分散固相萃取净化-超高效液相色谱-串联质谱法快速测定鱼虾中20种兽药残留的方法，这些兽药残留包括三类抗生素（磺胺类、喹诺酮类和氯霉素类）和两种三苯甲烷类（孔雀石绿（MG）和隐色孔雀石绿（LMG））。样品先用磷酸氢二钾溶液水解，然后用乙腈萃取。之后，萃取液用氯化钠脱水并盐析，再用旋转蒸发仪浓缩至近干。该残留物用1.0 mL甲醇溶解。所得溶液用C18和PSA吸附剂通过分散固相萃取法净化，并用滤膜过滤。目标化合物采用ZORBAX C18色谱柱进行分离。通过正、负离子模式的多反应监测（MRM）采集质谱数据，并采用同位素内标法进行定量。20种兽药在0.2 - 300 μg/L范围内呈现良好的线性关系。检测限和定量限分别为0.1 - 0.6 μg/kg和0.3 - 1.8 μg/kg，相关系数大于0.99。在三个加标水平（定量限的1、5和20倍）下的平均回收率在72.5% - 118%之间，相对标准偏差为1.9% - 9.8%。该方法的优点包括预处理简单、检测效率高、成本低。此外，它适用于同时测定鱼虾中的多种兽药残留。
