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目的采用超高效液相色谱-线性离子阱轨道离子阱组合式高分辨质谱联用技术(UPLC-LTQ Orbitrap MS),建立渔用中药制剂中氟喹诺酮类、磺胺类、四环素类、孔雀石绿类、硝基呋喃类以及喹噁啉类等48种西药成分的快速筛查与确证方法。方法样品经乙酸乙酯提取,C18吸附剂净化,经反相色谱柱分离,甲醇-水(含0.1%甲酸)为流动相梯度洗脱(流速250μl/min,柱温30℃,进样量10μl),通过LTQ Orbitrap MS全扫描,TOXID软件结合数据库检索,对48种西药成分进行快速筛查和确证。结果各化合物的检出限(LOD)为0.006 0～0.21 mg/kg;定量限(LOQ)为0.020～0.72 mg/kg,在线性范围内存在良好线性关系,相关系数r2为0.9796～0.9997;在0.25、0.50、1.00 mg/kg三个添加水平下,方法回收率分别为81.9%～114.4%、84.0%～114.3%、80.9%～114.8%,RSD为1.56%～14.3%。结论方法快速、准确、可靠、重现性好,可对中药基质中的部分违法添加药物进行筛查和确证。
Objective To establish fluoroquinolones, sulfonamides, tetracyclines and malachite green in fishery traditional Chinese medicine using ultra-high performance liquid chromatography-ion trap orbit ion trap combined with high resolution mass spectrometry (UPLC-LTQ Orbitrap MS) , Nitrofurans and quinoxaline and other 48 kinds of western medicine components of the rapid screening and confirmation method. Methods The sample was extracted with ethyl acetate and purified with C18 adsorbent. The residue was separated on a reversed phase column and eluted with a mobile phase of methanol-water (containing 0.1% formic acid) at a flow rate of 250 μl / min and a column temperature of 30 ° C. ), Through the LTQ Orbitrap MS full scan, TOXID software combined with database search, 48 kinds of western medicine components for rapid screening and confirmation. Results The limit of detection (LOD) of each compound ranged from 0.006 0 to 0.21 mg / kg. The limit of quantification (LOQ) ranged from 0.020 to 0.72 mg / kg with good linearity in the linear range. The correlation coefficient r2 was 0.9796 ~ 0.9997. The recovery rates were 81.9% ~ 114.4%, 84.0% ~ 114.3%, 80.9% ~ 114.8%, RSD 1.56% ~ 14.3% at the three levels of 0.25,0.50,1.00 mg / kg. Conclusion The method is rapid, accurate, reliable and reproducible. Some of the drugs in the matrix of traditional Chinese medicine can be illegally added for screening and confirmation.