超高效液相色谱-串联质谱法同时测定蜂蜜中4种抗病毒类药物残留

Simultaneous determination of 4 kinds of antiviral drug residues in honey by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  抗病毒药物  超高效液相色谱-串联质谱法  蜂蜜  残留

英文关键词:antiviral drugs  ultra performance liquid chromatography-tandem mass spectrometry  honey  residues

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)同时检测蜂蜜中金刚烷胺、金刚乙胺、吗啉胍和阿昔洛韦4种抗病毒药物残留的分析方法。方法 样品经20%乙腈水(含0.2%甲酸)溶液溶解, 超声提取后高速离心, 取上清液过Oasis PRiME HLB固相萃取柱净化, 净化后的样液进行上机测定; 选用SHISEIDO MGⅢ-H C18色谱柱(2.0 mm×100 mm, 3 μm), 以甲醇?0.1%甲酸水溶液为流动相进行梯度洗脱; 通过多反应监测, 在正离子模式下, 采用基质匹配外标法, 同时对4种化合物进行定性和定量分析。结果 金刚烷胺、金刚乙胺、吗啉胍和阿昔洛韦在各自浓度范围内线性关系良好, 相关系数均大于0.999。方法的检出限为0.2~1.0 μg/kg, 定量限为0.5~2.0 μg/kg; 在定量限、5、10、20 μg/kg 4个添加水平下的平均回收率为82.9%~93.5%, 相对标准偏差为2.0%~8.4% (n=6)。 结论 本方法简单、灵敏度高、重现性好, 适用于蜂蜜中4种抗病毒类药物的同时检测。

英文摘要:

      Objective To establish a method for simultaneous determination of amantadine, rimantadine, morpholine and acyclovir residues in honey by ultra performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS). Methods The samples were dissolved in 20% acetonitrile-water (containing 0.2% formic acid) solution, extracted by ultrasound, and centrifuged at high speed. The supernatant was purified by Oasis PRiME HLB solid-phase extraction column, and the purified sample liquid was tested on the computer. The Shiseido MG III-H C18 column (2.0 mm×100 mm, 3 μm) was used for gradient elution using methanol?0.1% formic acid aqueous solution as the mobile phase. Through multiple reaction monitoring, in the positive ion mode, the matrix matching external standard method was adopted, and the qualitative and quantitative analysis of 4 compounds was conducted simultaneously. Results The linear relationships of amantadine, rimantadine, moroxydine and acyclovir were good within the respective concentration ranges, and the correlation coefficients were all greater than 0.999. The limits of detection were 0.2?1.0 μg/kg, and the limits of quantitation were 0.5?2.0 μg/kg. The average recoveries were 82.9%?93.5% and the relative standard deviations were 2.0%?8.4% at the LOQ, 5, 10, and 20 μg/kg levels (n=6). Conclusion This method is simple, sensitive and reproducible, and is suitable for the simultaneous determination of 4 antiviral drugs in honey.