液相色谱-串联质谱法测定育肥猪配合饲料中的阿奇霉素

发布时间：2018-06-03 17:12

  本文选题：液相色谱-串联质谱(LC-MS/MS) + 阿奇霉素　； 参考：《分析测试学报》2017年03期

【摘要】：通过对提取溶剂、净化方法及色谱-质谱条件的优化,建立了配合饲料中阿奇霉素(AZM)的液相色谱-串联质谱测定方法。样品经乙腈超声波提取,MCX固相萃取柱净化,BDS Hypersil C_(18)(2.4μm,100 mm×2.1 mm)色谱柱分离,以甲醇-0.05 mol/L乙酸铵水溶液为流动相梯度洗脱,正离子模式电离,多反应监测模式检测,同位素内标法定量。在优化条件下,AZM在1~250μg/L范围内线性关系良好,相关系数(r~2)为0.999 1,检出限(S/N≥3)为2.8μg/kg,定量下限(S/N≥10)为8.4μg/kg;在0.5,1,5,10 mg/kg加标水平下,回收率为87.0%~106.6%,批内相对标准偏差为0.58%~5.4%,批间相对标准偏差为3.1%~5.4%。该方法准确、灵敏,选择性强,基质干扰小,可用于配合饲料中AZM的测定。
[Abstract]:A liquid chromatography-tandem mass spectrometry (LC-MS) method for the determination of azithromycin (AZM) in compound feed was established by optimizing the extraction solvent, purification method and chromatography-mass spectrometry conditions. The samples were purified by ultrasonic extraction with acetonitrile and purified on the column of BDS Hypersil (182.4 渭 m). The mobile phase gradient elution was methanol-0.05 mol/L ammonium acetate solution, the positive ion mode ionization, the multi-reaction monitoring mode detection and the isotope internal standard method. Under the optimized conditions, the linear range of AZM is 1: 250 渭 g / L, the correlation coefficient is 0.999 1, the detection limit S / N 鈮，

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