建立了基质固相分散-液相色谱法快速测定水产品中的孔雀石绿和结晶紫的新方法。将鱼肉样品粉碎后与C 18填料研磨混合，装柱、淋洗，洗脱液浓缩后用高效液相色谱检测。色谱条件：色谱柱Inertsil ODS-SP（5μm，4.6 mm×150 mm），乙腈和乙酸铵缓冲溶液体积比80∶20作流动相等度洗脱，流速1.00 mL/min，检测波长254 nm。结果表明，孔雀石绿和结晶紫在0.30μg/L~30.00μg/L范围内，线性关系良好，相关系数（r）均大于0.999，检测限（S/N=3）分别为：0.18 ng/g和1.10 ng/g，样品加标回收率分别为86.28%~98.79%和82.51%~93.71%，其精密度RSD均小于5%（n=5）。%A method for the determination of malachite green and crystal viole in aquatic products based on matrix solid-phase dispersion with liquid chromatography was established. Fish samples mix with C 18 after grinding, and then the blended material was transferred to a 6 mL SPE column. And then, the column was eluted with hexane, ethyl acetate and acetonitrile in sequential order. The eluent was collected and evaporated to dryness. The concentrated sample solution were filtrated with filter membrane(0.22μm),and then injected in to the HPLC system. The separation was carried on the inertsil ODS-SP (5 μm, 4.6 mm × 150 mm) chromatographic column with ammonium acetate/acetonitrile (80∶20) as mobile phase isocratic elution, and flow rate of 1.00 mL/min and the detection wavelength was 254 nm. The results show that, A good linearity (r>0.999) was achieved for the target compound over the range of 0.30μg/mL-30.00μg/mL. the limit of detection (S/N=3) of Calachite Green and Crystal Violer were 0.18 ng/g and 1.10 ng/g. the recoveries of Malachite Green and Crystal Violet from fish tissue ranged from 86.28%-98.79%and 82.51%-93.71%both with the relative standard deviations (RSD) within 5%.
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