QuEChERS-超高效液相色谱-质谱联用法分别测定禽蛋清和禽蛋黄中氯霉素类药物残留

Determination of chloramphenicoles residues in egg white and yolk by QuEChERS-ultra performance liquid chromatography-mass spectrometry

中文关键词:  超高效液相色谱-质谱联用法  QuEChERS  氯霉素类药物  禽蛋

英文关键词:ultra performance liquid chromatography-mass spectrometry  QuEChERS  chloramphenicoles residues  poultry egg

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-质谱联用法测定禽蛋清和禽蛋黄中氯霉素类药物残留的方法。方法 采用QuEChERS法进行样品前处理。样品经10 mL的乙腈提取, 除水, 净化, 氮吹浓缩, 0.5 mL 10%乙腈水复溶, 正己烷除脂后测定。待测溶液经C18色谱柱分离以0.01%氨水和甲醇为流动相进行梯度洗脱分离, 质谱检测采用电喷雾离子源正负离子切换和多反应监测扫描模式, 离子对、保留时间定性, 内标法定量。结果 在0.2~50 ng/mL范围内, 氯霉素类药物线性相关系数均大于0.999。当取样量是2.0 g时, 以3倍信噪比法计算的检出限为0.002~0.211 μg/kg。加标回收率为81%~122%, 相对标准偏差为1.6%~9.9% (n=6)。结论 本方法简便高效、灵敏度高、精密度好, 适用于禽蛋清和禽蛋黄中氯霉素类药物残留的检测, 可以满足日常检测的需要。

英文摘要:

      Objective To establish a method for determination of chloramphenicoles residues in poultry egg white and yolk by QuEChERS-ultra performance liquid chromatography-mass spectrometry. Methods The sample was pretreated by the QuEChERS method, extracted with 10 mL acetonitrile, dehydrated, purified, dissolved with 0.5 mL 10% acetonitrile after nitrogen blowing, degreased with hexane and then detected. The solution to be tested was separated on a C18 column by gradient elution with 0.01% ammonia and methanol as mobile phases. Electrospray ion source with positive and negative ion switching mode was applied and the data was acquired by multi-reaction monitoring scanning. The results were identified by ion pair and retention time, quantified by internal standard method. Results The linear of chloramphenicoles residues was from 0.2 to 50 ng/mL, with coefficients were all greater than 0.999. When the sampling volume was 2.0 g, the detection limits calculated by 3 times the signal-to-noise ratio method were 0.002-0.211 μg/kg, the recoveries were 81%-122%, and the relative standard deviations were 1.6%-9.9% (n=6). Conclusion This method is simple, efficient, with high sensitivity and precision, which is suitable for the detection of chloramphenicoles residues in poultry egg white and yolk and can meet the needs of daily detection.