高效液相色谱-串联质谱法测定牛奶中8种青霉素类药物

Determination of 8 penicillins antibiotics in milk by HPLC-MS/MS

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 the high performance liquid chromatography- mass spectrometry（ HPLC- MS / MS） for the determination of 8 penicillins antibiotics residue in milk. Methods The sample was extracted with ammoniac acetonitrile by an ultrasonic method. After concentrated with a rotary evaporator,the residue was defatted with n- hexane. The separation was performed on an C18 column utilizing a gradient elution program of acetonitrile and water（ containing 0. 1% formic acid and5 mmol ammonium acetate） as the mobile phase. It was then analyzed with HPLC- MS under the positive ion multiple reaction monitoring mode. Results The linear ranges were good from 2 μg / L to 200 μg / L with the correlation coefficients among0. 996 5- 0. 999 5 for all the 8 penicillins. The detection limits and the limits of quantitation were 0. 05 μg / kg- 2. 70 μg / kg and 0. 17 μg / kg- 8. 90 μg / kg respectively. The average recoveries of 8 penicillins were among 87. 8%- 108. 6% with the RSD of 7. 2%- 10. 8%. Conclusion This method need less time and reagents,it has high sensitivity and specificity. This method has been applied to the actual sample,and achieved satisfactory results.