超高效液相色谱-串联质谱法同时测定豆芽中18种抗菌剂的含量

Simultaneous determination of 18 kinds of antibacterial agents in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  固相萃取  抗菌剂  豆芽

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  antibacterial agents  bean sprouts

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定豆芽中18种抗菌剂的分析方法。方法 豆芽样品经乙酸乙酯:乙腈(1:1, V:V)提取, 提取液经盐析, 固相萃取柱净化, 采用Waters Acquity UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm), 以乙腈?0.3%甲酸水溶液为流动相分离目标物。电喷雾质谱正离子模式, 多反应监测模式检测, 外标法定量。结果 18种抗菌剂在1.0~50.0 ng/mL范围内线性关系良好, 相关系数(r)均大于0.99; 以黄豆芽和绿豆芽为基质, 进行3水平加标回收实验, 平均回收率为85.7%~107.5%, 相对标准偏差为0.1%~8.7% (n=6); 方法检出限在0.2~0.5 μg/kg之间, 方法定量限在0.7~1.7 μg/kg之间。结论 该方法检出限低、灵敏度高, 且具有较好的准确度和精密度, 可用于检测豆芽中18种抗菌剂的含量。

英文摘要:

      Objective To establish a method for the simultaneous determination of 18 kinds antibacterial agents in bean sprouts by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Bean sprout samples were extracted by ethyl acetate:acetonitrile (1:1, V:V), the extract was salted out and purified by solid phase extraction column, the target substances were separated on Waters Acquity UPLC HSS T3 column (100 mm× 2.1 mm, 1.8 μm), and gradient elution was performed with acetonitrile-0.3% formic acid aqueous solution as mobile phases. Multiple reaction monitoring mode was used for detection in electrospray ionization with positive ion mode, and external standard method was used for quantification. Results The 18 kinds of antibacterial agents had good linear relationships in the range of 1.0?50.0 ng/mL, and the correlation coefficients (r) was all greater than 0.99. Using soybean sprouts and mung bean sprouts as the matrix, 3 levels spiked recovery experiments were carried out, and the average recoveries were 85.7%?107.5%, and the relative standard deviations were 0.1%?8.7% (n=6); and the method detection limits were 0.2?0.5 μg/kg, and the method quantification limits were 0.7?1.7 μg/kg. Conclusion This method is highly sensitive, accurate, and has good reproducibility and stability, and can effectively detect the content of 18 kinds of antibacterial agents in bean sprouts.