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| 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喹诺酮类和苯二氮卓类药物 |
| Determination of multiple fluoroquinolones and benzodiazepines in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction purification |
| 投稿时间：2025-04-09 修订日期：2025-06-12 |
| DOI： |
| 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 |
| 基金项目:浙江省公益技术研究计划/分析测试项目(LGC20B050007)、浙江省“三农九方”科技协作计划项目(2023SNJF069) |
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| 中文摘要: |
| 摘要：目的 建立一种超高效液相色谱-串联质谱（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种苯二氮卓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)净化后直接上机分析，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 ng/mL浓度范围内线性良好，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（LOQs）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%~109.3%，相对标准偏差(RSDs)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种苯二氮卓类药物残留的高通量检测。 |
| 英文摘要: |
| ABSTRACT: Objective To establish an analytical method utilizing ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of six fluoroquinolones and four benzodiazepines residues in aquatic products. Methods Aquatic samples were extracted using 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). Following purification through a ProElut PLS-A solid phase extraction cartridge, the samples were analyzed directly by UPLC-MS/MS. Quantification was performed using the isotope internal standard method. Results The ten target compounds exhibited good linearity within the concentration range of 0.5 to 50 ng/mL, with correlation coefficients (r) all greater than 0.998. The limits of quantification (LOQs) for these compounds in five 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 109.3%, with relative standard deviations (RSDs) 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 six fluoroquinolones and four benzodiazepines residues in aquatic products. |
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