建立了QuEChERS(quick, easy, cheap, effective, rugged, safe)样品前处理技术结合超高效液相色谱-串联质谱法同时测定蜂蜜和蜂王浆中红霉素及其降解物残留的检测方法。样品用水溶解,经乙腈提取后,用N-丙基乙二胺和无水硫酸镁净化,以水溶液(含0.1%的甲酸,体积分数)和甲醇为流动相进行梯度洗脱,EC-C18色谱柱分离。采用多反应监测正离子模式扫描,基质标准曲线外标法定量。结果表明,该方法在0.2~100 ng/mL范围内线性关系良好,相关系数均大于0.99。方法检出限为0.2~0.63 μg/kg,定量限为0.5~1.9 μg/kg。该方法简单快速,可满足日常检测需要,可为蜂蜜和蜂王浆中的红霉素及其降解物的定性与定量检测提供参考依据。
A method for the simultaneous determination of erythromycin A and its degradation products in honey and royal jelly was established by using the pretreatment technology of QuEChERS (quick, easy, cheap, effective, rugged, safe) combined with ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The sample was dissolved in water, extracted with acetonitrile, and purified with primary secondary amine (PSA) and anhydrous magnesium sulfate powder. The aqueous solution (containing 0.1% of formic acid) and methanol was used as the mobile phase for gradient elution, and the analyte was separated on an EC-C18 column. Multiple reaction monitoring (MRM) positive ion mode scanning and matrix calibration cure external standard method was used for quantitative analysis. The results showed that the linear relationship was good in the range of 0.2-100 ng/mL, and the correlation coefficients was greater than 0.99. The detection limit of the method was 0.2-0.63 μg/kg, and the limit of quantification was 0.5-1.9 μg/kg. This method is simple and fast, which can meet the needs of routine analysis, and can be used to determine erythromycin A and its degradation products in honey and royal jelly.
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