不同基质食品中乌洛托品残留量的检测方法研究

Study on the determination method of urotropine residue in different food matrix

目的建立适用于猪肉、豆干、豆腐、腐竹基质中乌洛托品的分析检测方法。方法比较提取方式、浓缩温度、固相萃取柱、微孔滤膜等关键因素测定样品中乌洛托品,样品用乙腈超声提取,35℃旋蒸浓缩,经cleanert PCX固相萃取柱及0.22μm亲水PTFE微孔滤膜净化,高效液相色谱串联质谱仪进行检测。结果乌洛托品在5~500μg/L质量浓度范围内线性相关系数为0.9997;添加水平为1~50μg/kg时,平均回收率为75.7%~91.9%,相对标准偏差为1.10%~9.88%。结论该方法快速、准确度和精密度均能满足日常检测的需求。

Objective To establish an analytical method for the determination of urotropine in pork,bean curd,tofu and dried bean curd stick.Methods Key factors such as extraction method,concentration temperature,solid phase extraction column and microporous filtration membrane were compared and studied to determine the urlotropine content in the sample.The samples were extracted by ultrasonic extraction with acetonitrile and concentrated by rotary evaporation at 35℃,purified by cleanert PCX SPE column and 0.22μm hydrophilic PTFE microporous filtration membrane,and analyzed by high performance liquid chromatography tandem mass spectrometer.Results The correlation coefficient was 0.9997 at the concentration range 5‒500μg/L,and the average recoveries were 75.7%‒91.9%and the relative standard deviations(RSDs)were 1.10%‒9.88%when the supplemental levels were 1‒50μg/kg.Conclusion This method is rapid,accuracy and precision,and can meet the request of daily testing.