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目的建立水产品中孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫的高效液相色谱定量分析方法。方法对样品的提取方法,测定条件,方法的线性范围和精密度,准确度等进行实验。结果样品用乙腈直接提取,不加衍生试剂,不采用柱后衍生的方法,选用适宜的色谱柱在不同波长下同时测定样品中孔雀石绿、结晶紫、隐色孔雀石绿、隐色结晶紫的含量。在0μg/ml~10.0μg/ml范围内,浓度与峰面积呈直线相关关系;方法最低检出量为0.00020μg;按本法测定,最低检出浓度为0.0020 mg/kg。对加标量为0.025 mg/kg和0.050 mg/kg的样品,连续测定5次,相对标准偏差RSD为2.8%~9.1%,回收率为72%~96%。结论本法具有样品提取简单、稳定,测定简便、灵敏,结果精密、准确的特点,适用于水产品中孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫的测定。适合无液相色谱-质谱仪的基层单位推广应用。
Objective To establish a method for the quantitative analysis of malachite green, leucomalachite green, crystal violet and leuco crystal violet in aquatic products by high performance liquid chromatography. Methods The method of extraction, the determination conditions, the linear range and precision of the method, the accuracy and so on were tested. Results The samples were directly extracted with acetonitrile, without derivatization reagent, no post-column derivatization method, and the appropriate column was used to determine the concentration of malachite green, crystal violet, leucomalachite green, leuco crystal violet Content. In the range of 0μg / ml ~ 10.0μg / ml, there is a linear correlation between the concentration and the peak area; the minimum detectable quantity is 0.00020μg; the minimum detectable concentration is 0.0020 mg / kg according to this method. The results showed that the relative standard deviations (RSDs) were 2.8% ~ 9.1% and the recoveries were 72% ~ 96% for 5 consecutive determinations of spiked samples at 0.025 mg / kg and 0.050 mg / kg. Conclusion The method is simple, stable, simple, sensitive, precise and accurate. It is suitable for the determination of malachite green, leucomalachite green, crystal violet and leuco crystal violet in aquatic products. Suitable for non-liquid chromatography-mass spectrometer of the promotion and application of grassroots units.