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目的建立一种高效液相色谱-串联质谱(HPLC-MS/MS)法快速测定牛奶中8种青霉素类药物残留的检测方法。方法样品经氨化乙腈超声提取,旋蒸浓缩,正己烷脱脂,经C18色谱柱分离,以乙腈-5 mmol/L乙酸铵(含0.1%甲酸)溶液为流动相进行梯度洗脱,最后采用高效液相色谱-串联质谱法在正离子多反应监测模式下测定。结果 8种青霉素类药物在2μg/L~200μg/L时具有良好的线性关系,相关系数(r)为0.996 5~0.999 5,检出限和定量限分别为0.05μg/kg~2.70μg/kg和0.17μg/kg~8.90μg/kg;方法的回收率为87.8%~108.6%,相对标准偏差(RSD)为7.2%~10.8%。结论该法具有耗时短、试剂使用少、灵敏度高、特异性强等特点,已应用于实际样品的检测,并取得满意结果。
OBJECTIVE To establish a HPLC-MS / MS method for rapid determination of 8 penicillin residues in milk. Methods The sample was extracted by ammoniacal acetonitrile, concentrated by rotary evaporation and degreased by hexane. The residue was separated by C18 column and eluted with 5 mmol / L ammonium acetate (containing 0.1% formic acid) as mobile phase. Liquid chromatography - tandem mass spectrometry in positive ion multiple reaction monitoring mode. Results There were good linear relationships between 8 kinds of penicillins and 2μg / L ~ 200μg / L, the correlation coefficient (r) was 0.996 5 ~ 0.999 5, and the limits of detection and limit of quantification were 0.05μg / kg ~ 2.70μg / kg And 0.17 μg / kg ~ 8.90 μg / kg, respectively. The recoveries of the method were 87.8% -108.6% with relative standard deviations (RSDs) of 7.2% -10.8%. Conclusion The method has the characteristics of short time-consuming, less reagent, high sensitivity and specificity. It has been applied to the detection of real samples and obtained satisfactory results.