QuEChERS-高效液相色谱-串联质谱法测定禽蛋中10种氨基糖苷类药物残留

Determination of 10 kinds of aminoglycosides residues in poultry eggs by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

目的建立了利用QuEChERS净化高效液相色谱-串联质谱法同时检测禽蛋中10种氨基糖苷类药物(潮霉素B、阿米卡星、安普霉素、卡那霉素、庆大霉素C1、庆大霉素C1a、庆大霉素C2、巴龙霉素、西索米星、奈替米星)残留的方法。方法样品经5%(V/V)三氯乙酸振摇提取,QuEChERS净化,采用Amide高效液相色谱柱分离,以1%(V/V)甲酸水和90%(V/V)乙腈水进行梯度洗脱,外标法定量。结果在20~1000μg/L质量浓度范围内线性关系良好,相关系数均大于0.99,方法的检出限为0.2 mg/kg,定量限为0.5 mg/kg,对各种基质进行1、2、10倍定量限进行3水平的加标实验,平均回收率为63.6%~119.0%(n=6),相对标准偏差为1.0%~7.5%。利用该方法对市场销售的鸡蛋、鹅蛋、鹌鹑蛋各20批次进行检测,均未检出氨基糖苷类化合物。结论该方法利用QuEChERS净化可以更简便、快速、准确的实现禽蛋中10种氨基糖苷类药物残留的检测。

Objective To establish a method for the simultaneous determination of 10 kinds of aminoglycosides(hygromycin B,amikacin,apramycin,kanamycin,gentamycin C1,gentamycin C1a,gentamycin C2,paromomycin,sisomicin and netilmicin)residues in poultry eggs by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted by shaking with 5%(V/V)trichloroacetic acid,purified by the QuEChERS method,separated by Amide high performance liquid chromatography column.Meanwhile,gradient elution was carried out with 1%(V/V)formic acid water and 90%(V/V)acetonitrile in water as mobile phase,which quantified by the external standard method.Results The linear relationships were pretty good when the mass concentration was 20–1000μg/L.The correlation coefficients were all above 0.99.The limits of detection were 0.2 mg/kg,and the limits of quantitation were 0.5 mg/kg.Various matrices were tested 1,2,10 quantitation limit for 3 levels of spiking experiments,the average recoveries were 63.6%–119.0%(n=6),and the relative standard deviations were 1.0%–7.5%.This method was used to test 20 batches of eggs,goose eggs,and quail eggs sold on the market,and no aminoglycosides were detected in any of them.Conclusion Using QuEChERS purification method,the detection of 10 kinds of aminoglycosides residues in poultry eggs can be realized more simply,quickly and accurately.