通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中多种氟喹诺酮类和苯二氮䓬类药物

Determination of multiple fluoroquinolones and benzodiazepines in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction

中文关键词:  氟喹诺酮，苯二氮卓，水产品，通过式固相萃取

英文关键词:fluoroquinolones  benzodiazepines  aquatic products  pass-through solid phase extraction

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法(ultra-performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定水产品中6种氟喹诺酮类和4种苯二氮?类药物残留的分析方法。方法 使用1%甲酸乙腈溶液对水产样品进行提取, 提取液经旋转蒸发仪浓缩后用90%乙腈水溶液(含1%甲酸)复溶, 经通过式固相萃取小柱(ProElut PLS-A)净化后直接供UPLC-MS/MS分析, 采用同位素内标法进行定量。结果 10种目标化合物在0.5~50.0 ng/mL质量浓度范围内线性关系良好, 相关系数(r)均大于0.998。10种目标化合物在5种水产品基质中定量限为0.5~1.0 μg/kg, 低、中、高3个不同水平的加标回收率范围为81.5%~109.7%, 相对标准偏差为0.24%~13.22%。结论 经方法学验证, 该方法灵敏度高、定量准确、稳定性好、操作简单高效, 可用于水产品中6种氟喹诺酮类和4种苯二氮?类药物残留的高通量检测。

英文摘要:

      Objective To establish an analytical method for the simultaneous determination of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Aquatic product samples were extracted with 1% formic acid in acetonitrile. The extracts were concentrated with a rotary evaporator and then reconstituted in 90% acetonitrile aqueous solution (containing 1% formic acid), and purified through a pass-through solid phase extraction cartridge (ProElut PLS-A). The purified extracts were directly analyzed by UPLC-MS/MS. Quantification was performed using the isotope internal standard method. Results The 10 kinds of target compounds exhibited good linearity within the concentration range of 0.5 to 50.0 ng/mL, with correlation coefficients (r) all greater than 0.998. The limits of quantitation for these compounds in 5 kinds of different aquatic product matrices ranged from 0.5 to 1.0 μg/kg. The recovery rates at low, medium and high spiking levels ranged from 81.5% to 109.7%, with relative standard deviations ranging from 0.24% to 13.22%. Conclusion Methodological validation confirmed that the developed method is highly sensitive, accurate in quantification, stable, and straightforward in operation. It is suitable for high-throughput detection of 6 kinds of fluoroquinolones and 4 kinds of benzodiazepines residues in aquatic products.