超高液相色谱-串联质谱法测定水产品中氯霉素残留量

Determination of Chloramphenicol Residues in Aquatic Products by Ultra High Liquid Chromatography Tandem Mass Spectrometry

目的:建立超高效液相色谱-串联质谱法测定水产品中氯霉素残留量的分析方法。方法:样品用氨化乙酸乙酯超声振荡提取,提取液蒸干后用水复溶,采用电喷雾离子化,负离子扫描和多反映监测模式(Multi reaction monitor,MRM)检测,内标法定量。实验探讨和优化了提取溶剂用量及浓缩方式等前处理方法,并优化检测方法的色谱、质谱条件。结果:在0.1~10 ng·mL^-1范围内线性相关系数Y=0.993 635X-0.026 6435,相关系数r为0.999 2;方法检出限为0.02μg·kg^-1;在0.1~1.0μg·kg^-1浓度梯度范围内的平均回收率为97.2%~99.8%;变异系数在1.1%~3.0%。结论:该方法简便、经济、快捷、稳定、准确性高,能满足快速测定大批量水产品中氯霉素残留量的要求。

Objective: A method for the determination of chloramphenicol residues in aquatic products by ultra high performance liquid chromatography tandem mass spectrometry was established. Methods: The samples were extracted by ultrasonic vibration with ammoniated ethyl acetate. The extract was evaporated and then dissolved in water. Electrospray ionization, negative ion scanning and multi reaction monitor(MRM) were used to detect the content. The internal standard method was used to quantify the sample. The pretreatment methods, such as the amount of extraction solvent and the way of concentration, were studied and optimized, and the conditions of chromatography and mass spectrometry were optimized. Results: The linear correlation coefficient y=0.993 635 x-0.026 643 5 in the range of 0.1 ~ 10 ng·mL^-1, and the correlation coefficient r is 0.999 2. The detection limit of four nitrofuran metabolites ranged 0.02 μg·kg^-1. The average recoveries for nitrofuran metabolites were 97.2% ~ 99.8%;respectively, and their relative standard deviation varied between 1.1% ~ 3.0%. Conclusion: The method is simple, economic, fast, stable and accurate, which can meet the requirements of rapid determination of chloramphenicol residues in large quantities of aquatic products.